# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 2017

####################################################################### 
# 
# 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_zxg-zhx-3-100k
_database_code_depnum_ccdc_archive 'CCDC 1504830'
_audit_update_record             
;
2016-09-18 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_audit_creation_date             2016-05-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H8 Cl2 N1.33 O, C9 H7.78 Cl2 N1.33 O'
_chemical_formula_sum            'C18 H16 Cl4 N4 O2'
_chemical_formula_weight         462.15
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   14.7047(4)
_cell_length_b                   14.7047(4)
_cell_length_c                   23.9058(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4476.6(3)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    5051
_cell_measurement_temperature    103(4)
_cell_measurement_theta_max      72.3940
_cell_measurement_theta_min      5.0740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45790
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10167
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        66.911
_diffrn_reflns_theta_max         66.911
_diffrn_reflns_theta_min         5.075
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -35.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -19.0000   60.0000 101

#__ type_ start__ end____ width___ exp.time_
  2 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   57.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921 -125.0000 -180.0000 67

#__ type_ start__ end____ width___ exp.time_
  4 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921 -125.0000    0.0000 67

#__ type_ start__ end____ width___ exp.time_
  5 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  6 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -77.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  7 omega   17.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   38.0000 -120.0000 88

#__ type_ start__ end____ width___ exp.time_
  8 omega   38.00  116.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 78

#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  109.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 70

#__ type_ start__ end____ width___ exp.time_
 11 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
 12 omega   40.00  135.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
 13 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
 14 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

#__ type_ start__ end____ width___ exp.time_
 15 omega   70.00  178.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

#__ type_ start__ end____ width___ exp.time_
 16 omega   46.00  104.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
 17 omega   99.00  171.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 72

#__ type_ start__ end____ width___ exp.time_
 18 omega   46.00  121.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -180.0000 75

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00   68.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 30

#__ type_ start__ end____ width___ exp.time_
 20 omega   45.00  115.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 70

#__ type_ start__ end____ width___ exp.time_
 21 omega   91.00  116.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   45.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0798216000
_diffrn_orient_matrix_UB_12      0.0566787000
_diffrn_orient_matrix_UB_13      0.0473305000
_diffrn_orient_matrix_UB_21      -0.0349520000
_diffrn_orient_matrix_UB_22      0.0826967000
_diffrn_orient_matrix_UB_23      0.0033335000
_diffrn_orient_matrix_UB_31      -0.0838585000
_diffrn_orient_matrix_UB_32      -0.0677194000
_diffrn_orient_matrix_UB_33      0.0436214000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.730
_reflns_Friedel_fraction_max     0.730
_reflns_number_gt                3063
_reflns_number_total             3102
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 
;
 Flack x determined using 1189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.360(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3102
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0700
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1330P)²+20.4400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.1915
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Sof(Cl)=1-FVAR(1)
 Sof(Cl04)=Sof(H00Q)=FVAR(1)
 Sof(Cl1)=1-FVAR(2)
 Sof(Cl02)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C00J(H00H,H00J), C00K(H00K,H00M), C00M(H00A,H00B), C00R(H00C,H00D)
3.b Aromatic/amide H refined with riding coordinates:
 C00A(H00E), C00C(H00F), C00E(H00G), C00I(H00I), C00L(H00L), C00Q(H00Q)
3.c Idealised tetrahedral OH refined as rotating group:
 O005(H005), O006(H006)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl01 Cl 1.05146(11) 0.43044(12) 0.34917(8) 0.0370(4) Uani 1 1 d . . . . .
Cl02 Cl 0.29259(12) 0.21630(13) 0.65673(8) 0.0250(4) Uani 0.832(4) 1 d . . . A
1
Cl03 Cl 0.77595(12) 0.51761(14) 0.44816(7) 0.0393(4) Uani 1 1 d . . . . .
Cl04 Cl 0.63478(17) 0.52057(18) 0.55308(9) 0.0409(6) Uani 0.784(5) 1 d . . . A
1
O005 O 0.9647(3) 0.4604(3) 0.2451(2) 0.0283(9) Uani 1 1 d . . . . .
H005 H 0.9260 0.4478 0.2180 0.042 Uiso 1 1 calc GR . . . .
O006 O 0.4118(4) 0.3067(4) 0.7593(2) 0.0353(12) Uani 1 1 d . . . . .
H006 H 0.3984 0.2454 0.7590 0.053 Uiso 1 1 calc GR . . . .
N007 N 0.8442(3) 0.5009(4) 0.1875(2) 0.0221(11) Uani 1 1 d . . . . .
C008 C 0.8377(4) 0.4966(4) 0.2870(3) 0.0194(12) Uani 1 1 d . . . . .
N009 N 0.6667 0.3333 0.8863(3) 0.0188(17) Uani 1 3 d S T P . .
C00A C 0.9063(4) 0.4740(4) 0.3918(3) 0.0219(13) Uani 1 1 d . . . . .
H00E H 0.9282 0.4650 0.4269 0.026 Uiso 1 1 calc R . . . .
C00B C 0.9193(4) 0.4726(4) 0.2904(3) 0.0201(12) Uani 1 1 d . . . . .
C00C C 0.7936(4) 0.5096(4) 0.3355(3) 0.0225(13) Uani 1 1 d . . . . .
H00F H 0.7400 0.5256 0.3333 0.027 Uiso 1 1 calc R . . . .
N00D N 0.6667 0.3333 0.1170(4) 0.0248(19) Uani 1 3 d S T P . .
C00E C 0.8039(4) 0.5104(4) 0.2323(3) 0.0203(12) Uani 1 1 d . . . . .
H00G H 0.7506 0.5269 0.2300 0.024 Uiso 1 1 calc R . . . .
C00F C 0.9516(4) 0.4624(4) 0.3438(3) 0.0230(13) Uani 1 1 d . . . . .
N00G N 0.5730(4) 0.4365(4) 0.8142(3) 0.0348(14) Uani 1 1 d . . . . .
C00H C 0.8292(4) 0.4989(4) 0.3871(3) 0.0237(14) Uani 1 1 d . . . . .
C00I C 0.6192(4) 0.4767(4) 0.7705(3) 0.0237(13) Uani 1 1 d . . . . .
H00I H 0.6883 0.5315 0.7721 0.028 Uiso 1 1 calc R . . . .
C00J C 0.7681(4) 0.4180(4) 0.0976(2) 0.0215(12) Uani 1 1 d . . . . .
H00H H 0.7608 0.4352 0.0593 0.026 Uiso 1 1 calc R . . . .
H00J H 0.8183 0.3935 0.0978 0.026 Uiso 1 1 calc R . . . .
C00K C 0.8107(5) 0.5164(4) 0.1328(3) 0.0280(14) Uani 1 1 d . . . . .
H00K H 0.8698 0.5738 0.1138 0.034 Uiso 1 1 calc R . . . .
H00M H 0.7568 0.5355 0.1375 0.034 Uiso 1 1 calc R . . . .
C00L C 0.6181(5) 0.4879(5) 0.6669(3) 0.0323(15) Uani 1 1 d . . . . .
H00L H 0.6860 0.5448 0.6688 0.039 Uiso 1 1 calc R . . . .
C00M C 0.6242(4) 0.4749(4) 0.8688(3) 0.0288(15) Uani 1 1 d . . . . .
H00A H 0.5945 0.5125 0.8876 0.035 Uiso 1 1 calc R . . . .
H00B H 0.6987 0.5226 0.8636 0.035 Uiso 1 1 calc R . . . .
C00N C 0.5680(5) 0.4402(5) 0.7144(3) 0.0316(15) Uani 1 1 d . . . . .
C00O C 0.4640(5) 0.3547(5) 0.7125(3) 0.0316(15) Uani 1 1 d . . . . .
C00P C 0.4199(5) 0.3217(5) 0.6598(3) 0.0338(16) Uani 1 1 d . . . . .
C00Q C 0.4705(6) 0.3694(5) 0.6109(3) 0.0364(15) Uani 1 1 d . . . . .
H00Q H 0.4380 0.3450 0.5764 0.044 Uiso 0.784(5) 1 calc R . . A 1
C00R C 0.6071(5) 0.3825(6) 0.9034(3) 0.0372(17) Uani 1 1 d . . . . .
H00C H 0.6248 0.4052 0.9419 0.045 Uiso 1 1 calc R . . . .
H00D H 0.5331 0.3301 0.9023 0.045 Uiso 1 1 calc R . . . .
C00S C 0.5692(5) 0.4531(6) 0.6144(4) 0.0417(18) Uani 1 1 d . . . . .
Cl Cl 0.5678(7) 0.4503(7) 0.5633(4) 0.046(2) Uani 0.216(5) 1 d . . . A 2
Cl1 Cl 0.3184(7) 0.2683(7) 0.6551(5) 0.032(2) Uani 0.168(4) 1 d . . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl01 C00F 1.756(6) . ?
Cl02 C00P 1.735(6) . ?
Cl03 C00H 1.743(7) . ?
Cl04 C00S 1.763(8) . ?
O005 H005 0.8200 . ?
O005 C00B 1.331(8) . ?
O006 H006 0.8200 . ?
O006 C00O 1.340(8) . ?
N007 C00E 1.265(8) . ?
N007 C00K 1.454(8) . ?
C008 C00B 1.412(8) . ?
C008 C00C 1.388(9) . ?
C008 C00E 1.450(9) . ?
N009 C00R 1.445(8) 2_655 ?
N009 C00R 1.445(8) . ?
N009 C00R 1.445(8) 3_665 ?
C00A H00E 0.9300 . ?
C00A C00F 1.381(9) . ?
C00A C00H 1.359(9) . ?
C00B C00F 1.395(9) . ?
C00C H00F 0.9300 . ?
C00C C00H 1.378(9) . ?
N00D C00J 1.460(6) 3_665 ?
N00D C00J 1.460(6) . ?
N00D C00J 1.460(6) 2_655 ?
C00E H00G 0.9300 . ?
N00G C00I 1.226(9) . ?
N00G C00M 1.470(9) . ?
C00I H00I 0.9300 . ?
C00I C00N 1.499(10) . ?
C00J H00H 0.9700 . ?
C00J H00J 0.9700 . ?
C00J C00K 1.514(8) . ?
C00K H00K 0.9700 . ?
C00K H00M 0.9700 . ?
C00L H00L 0.9300 . ?
C00L C00N 1.344(10) . ?
C00L C00S 1.410(11) . ?
C00M H00A 0.9700 . ?
C00M H00B 0.9700 . ?
C00M C00R 1.501(10) . ?
C00N C00O 1.414(8) . ?
C00O C00P 1.390(10) . ?
C00P C00Q 1.375(11) . ?
C00P Cl1 1.298(12) . ?
C00Q H00Q 0.9300 . ?
C00Q C00S 1.357(10) . ?
C00Q Cl 1.747(12) . ?
C00Q Cl1 2.237(12) . ?
C00R H00C 0.9700 . ?
C00R H00D 0.9700 . ?
C00S Cl 1.222(12) . ?

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
C00B O005 H005 109.5 . . ?
C00O O006 H006 109.5 . . ?
C00E N007 C00K 121.9(6) . . ?
C00B C008 C00E 118.7(5) . . ?
C00C C008 C00B 120.1(6) . . ?
C00C C008 C00E 121.2(5) . . ?
C00R N009 C00R 112.3(4) 3_665 . ?
C00R N009 C00R 112.3(4) 2_655 3_665 ?
C00R N009 C00R 112.3(4) 2_655 . ?
C00F C00A H00E 120.6 . . ?
C00H C00A H00E 120.6 . . ?
C00H C00A C00F 118.8(6) . . ?
O005 C00B C008 122.2(6) . . ?
O005 C00B C00F 120.6(6) . . ?
C00F C00B C008 117.1(6) . . ?
C008 C00C H00F 120.0 . . ?
C00H C00C C008 120.0(6) . . ?
C00H C00C H00F 120.0 . . ?
C00J N00D C00J 110.4(4) . 2_655 ?
C00J N00D C00J 110.4(4) 3_665 . ?
C00J N00D C00J 110.4(4) 3_665 2_655 ?
N007 C00E C008 122.4(6) . . ?
N007 C00E H00G 118.8 . . ?
C008 C00E H00G 118.8 . . ?
C00A C00F Cl01 119.4(5) . . ?
C00A C00F C00B 122.5(6) . . ?
C00B C00F Cl01 118.0(5) . . ?
C00I N00G C00M 121.2(5) . . ?
C00A C00H Cl03 118.3(5) . . ?
C00A C00H C00C 121.5(6) . . ?
C00C C00H Cl03 120.3(5) . . ?
N00G C00I H00I 118.9 . . ?
N00G C00I C00N 122.1(5) . . ?
C00N C00I H00I 118.9 . . ?
N00D C00J H00H 108.9 . . ?
N00D C00J H00J 108.9 . . ?
N00D C00J C00K 113.4(5) . . ?
H00H C00J H00J 107.7 . . ?
C00K C00J H00H 108.9 . . ?
C00K C00J H00J 108.9 . . ?
N007 C00K C00J 111.2(5) . . ?
N007 C00K H00K 109.4 . . ?
N007 C00K H00M 109.4 . . ?
C00J C00K H00K 109.4 . . ?
C00J C00K H00M 109.4 . . ?
H00K C00K H00M 108.0 . . ?
C00N C00L H00L 119.5 . . ?
C00N C00L C00S 121.0(6) . . ?
C00S C00L H00L 119.5 . . ?
N00G C00M H00A 110.0 . . ?
N00G C00M H00B 110.0 . . ?
N00G C00M C00R 108.6(5) . . ?
H00A C00M H00B 108.3 . . ?
C00R C00M H00A 110.0 . . ?
C00R C00M H00B 110.0 . . ?
C00L C00N C00I 121.5(5) . . ?
C00L C00N C00O 120.2(7) . . ?
C00O C00N C00I 118.3(6) . . ?
O006 C00O C00N 121.4(7) . . ?
O006 C00O C00P 121.9(6) . . ?
C00P C00O C00N 116.7(6) . . ?
C00O C00P Cl02 117.2(5) . . ?
C00Q C00P Cl02 119.1(6) . . ?
C00Q C00P C00O 123.7(6) . . ?
Cl1 C00P C00O 119.0(8) . . ?
Cl1 C00P C00Q 113.6(8) . . ?
C00P C00Q H00Q 121.0 . . ?
C00P C00Q Cl 161.9(7) . . ?
C00P C00Q Cl1 32.1(4) . . ?
C00S C00Q C00P 118.0(7) . . ?
C00S C00Q H00Q 121.0 . . ?
C00S C00Q Cl 44.2(5) . . ?
C00S C00Q Cl1 146.5(7) . . ?
Cl C00Q Cl1 165.1(6) . . ?
N009 C00R C00M 115.4(6) . . ?
N009 C00R H00C 108.4 . . ?
N009 C00R H00D 108.4 . . ?
C00M C00R H00C 108.4 . . ?
C00M C00R H00D 108.4 . . ?
H00C C00R H00D 107.5 . . ?
C00L C00S Cl04 120.0(5) . . ?
C00Q C00S Cl04 119.6(6) . . ?
C00Q C00S C00L 120.3(7) . . ?
Cl C00S C00L 154.1(8) . . ?
Cl C00S C00Q 85.1(7) . . ?
C00S Cl C00Q 50.7(5) . . ?
C00P Cl1 C00Q 34.3(5) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-05-10
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zxg-zxh-01
_database_code_depnum_ccdc_archive 'CCDC 1504826'
_audit_update_record             
;
2016-09-18 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_audit_creation_date             2016-05-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H30 N4 O3'
_chemical_formula_sum            'C27 H30 N4 O3'
_chemical_formula_weight         458.55
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.8325(10)
_cell_length_b                   11.2257(10)
_cell_length_c                   22.882(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.783(9)
_cell_angle_gamma                90
_cell_volume                     2496.0(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3920
_cell_measurement_temperature    292.76(15)
_cell_measurement_theta_max      26.3330
_cell_measurement_theta_min      3.6400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60630
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.6
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15165
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.477
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.76(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -9.00  100.00   1.0000    5.6900
omega____ theta____ kappa____ phi______ frames
    -       25.8970   57.0000  -60.0000 109

#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   61.00   1.0000    5.6900
omega____ theta____ kappa____ phi______ frames
    -       25.8970  -57.0000  120.0000 109

#__ type_ start__ end____ width___ exp.time_
  3 omega   35.00  116.00   1.0000    5.6900
omega____ theta____ kappa____ phi______ frames
    -       25.8970  178.0000  -30.0000 81

#__ type_ start__ end____ width___ exp.time_
  4 omega  -20.00   26.00   1.0000    5.6900
omega____ theta____ kappa____ phi______ frames
    -      -26.8345  -99.0000  -90.0000 46

#__ type_ start__ end____ width___ exp.time_
  5 omega  -20.00   26.00   1.0000    5.6900
omega____ theta____ kappa____ phi______ frames
    -      -26.8345  -99.0000   60.0000 46

#__ type_ start__ end____ width___ exp.time_
  6 omega  -54.00   -4.00   1.0000    5.6900
omega____ theta____ kappa____ phi______ frames
    -       25.8970  -38.0000  -60.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0242989000
_diffrn_orient_matrix_UB_12      0.0545330000
_diffrn_orient_matrix_UB_13      -0.0134722000
_diffrn_orient_matrix_UB_21      0.0673262000
_diffrn_orient_matrix_UB_22      0.0240410000
_diffrn_orient_matrix_UB_23      0.0060049000
_diffrn_orient_matrix_UB_31      0.0137728000
_diffrn_orient_matrix_UB_32      -0.0212310000
_diffrn_orient_matrix_UB_33      -0.0276900000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3332
_reflns_number_total             5097
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5097
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0795
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0990P)²+0.2170P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.2045
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 C00G, C00J
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C00G \\sim C00J: within 2A with sigma of 0.007 and sigma for terminal atoms of
0.001
4.a Secondary CH2 refined with riding coordinates:
 C00K(H00a,H00b), C00N(H00c,H00g), C00O(H00h,H00k), C00P(H00n,H00o), C00T(H00p,
 H00t), C00U(H00u,H00v)
4.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00D(H00D), C00E(H00E), C00F(H00F), C00I(H00I), C00J(H00J),
 C00L(H00L), C00M(H00M), C00Q(H00Q), C00R(H00R), C00S(H00S), C00V(H00w),
 C00W(H00x), C00X(H00y), C00Y(H00z)
4.c Idealised tetrahedral OH refined as rotating group:
 O001(H001), O002(H002), O003(H003)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O001 O 0.04277(16) 0.43540(17) 0.43113(8) 0.0854(5) Uani 1 1 d . . . . .
H001 H 0.0668 0.4964 0.4496 0.128 Uiso 1 1 calc GR . . . .
O002 O 0.1756(2) 0.87372(15) 0.23851(8) 0.0862(5) Uani 1 1 d . . . . .
H002 H 0.1270 0.8744 0.2646 0.129 Uiso 1 1 calc GR . . . .
O003 O 0.6375(2) 0.76684(18) 0.47243(7) 0.0944(6) Uani 1 1 d . . . . .
H003 H 0.5812 0.8213 0.4684 0.142 Uiso 1 1 calc GR . . . .
N004 N 0.4447(2) 0.90324(16) 0.41889(8) 0.0694(5) Uani 1 1 d . . . . .
N005 N 0.1586(2) 0.86860(16) 0.44758(8) 0.0707(5) Uani 1 1 d . . . . .
N006 N 0.2056(2) 0.60151(18) 0.47528(8) 0.0719(5) Uani 1 1 d . . . . .
N007 N 0.05179(19) 0.78996(19) 0.32045(9) 0.0726(5) Uani 1 1 d . . . . .
C008 C 0.54677(19) 0.74706(18) 0.36997(8) 0.0536(5) Uani 1 1 d . . . . .
C009 C 0.4480(2) 0.84331(19) 0.37252(10) 0.0603(5) Uani 1 1 d . . . . .
H009 H 0.3855 0.8610 0.3389 0.072 Uiso 1 1 calc R . . . .
C00A C 0.6384(2) 0.71240(19) 0.42001(9) 0.0598(5) Uani 1 1 d . . . . .
C00B C 0.2724(2) 0.4559(2) 0.40997(10) 0.0650(6) Uani 1 1 d . . . . .
C00C C 0.1442(2) 0.3979(2) 0.40311(10) 0.0675(6) Uani 1 1 d . . . . .
C00D C 0.2976(3) 0.5597(2) 0.44834(10) 0.0703(6) Uani 1 1 d . . . . .
H00D H 0.3836 0.5959 0.4531 0.084 Uiso 1 1 calc R . . . .
C00E C 0.5524(2) 0.6872(2) 0.31754(10) 0.0691(6) Uani 1 1 d . . . . .
H00E H 0.4919 0.7085 0.2839 0.083 Uiso 1 1 calc R . . . .
C00F C 0.7345(2) 0.5647(2) 0.36380(12) 0.0717(6) Uani 1 1 d . . . . .
H00F H 0.7983 0.5043 0.3616 0.086 Uiso 1 1 calc R . . . .
C00G C 0.1646(2) 0.6646(2) 0.25943(10) 0.0680(6) Uani 1 1 d . U . . .
C00H C 0.2073(2) 0.7604(2) 0.22673(10) 0.0687(6) Uani 1 1 d . . . . .
C00I C 0.7303(2) 0.6202(2) 0.41606(11) 0.0685(6) Uani 1 1 d . . . . .
H00I H 0.7896 0.5962 0.4496 0.082 Uiso 1 1 calc R . . . .
C00J C 0.0867(2) 0.6858(2) 0.30676(11) 0.0721(6) Uani 1 1 d . U . . .
H00J H 0.0610 0.6212 0.3280 0.087 Uiso 1 1 calc R . . . .
C00K C 0.3407(3) 0.9959(2) 0.41876(12) 0.0813(7) Uani 1 1 d . . . . .
H00A H 0.2849 1.0002 0.3800 0.098 Uiso 1 1 calc R . . . .
H00B H 0.3852 1.0724 0.4271 0.098 Uiso 1 1 calc R . . . .
C00L C 0.6456(2) 0.5966(2) 0.31402(11) 0.0763(7) Uani 1 1 d . . . . .
H00L H 0.6482 0.5576 0.2783 0.092 Uiso 1 1 calc R . . . .
C00M C 0.1224(3) 0.2994(2) 0.36604(12) 0.0858(8) Uani 1 1 d . . . . .
H00M H 0.0381 0.2603 0.3617 0.103 Uiso 1 1 calc R . . . .
C00N C 0.0312(3) 0.9049(3) 0.40967(13) 0.0903(8) Uani 1 1 d . . . . .
H00C H 0.0496 0.9739 0.3866 0.108 Uiso 1 1 calc R . . . .
H00G H -0.0365 0.9276 0.4343 0.108 Uiso 1 1 calc R . . . .
C00O C -0.0270(3) 0.8059(3) 0.36822(13) 0.0879(8) Uani 1 1 d . . . . .
H00H H -0.0269 0.7321 0.3903 0.105 Uiso 1 1 calc R . . . .
H00K H -0.1216 0.8245 0.3520 0.105 Uiso 1 1 calc R . . . .
C00P C 0.2504(3) 0.9690(2) 0.46466(13) 0.0865(8) Uani 1 1 d . . . . .
H00N H 0.3078 0.9512 0.5020 0.104 Uiso 1 1 calc R . . . .
H00O H 0.1959 1.0389 0.4704 0.104 Uiso 1 1 calc R . . . .
C00Q C 0.2844(3) 0.7388(3) 0.18249(11) 0.0853(8) Uani 1 1 d . . . . .
H00Q H 0.3122 0.8020 0.1608 0.102 Uiso 1 1 calc R . . . .
C00R C 0.3731(3) 0.4122(3) 0.37979(13) 0.0867(8) Uani 1 1 d . . . . .
H00R H 0.4589 0.4489 0.3845 0.104 Uiso 1 1 calc R . . . .
C00S C 0.2028(3) 0.5499(2) 0.24566(14) 0.0903(8) Uani 1 1 d . . . . .
H00S H 0.1749 0.4855 0.2665 0.108 Uiso 1 1 calc R . . . .
C00T C 0.2337(3) 0.7021(2) 0.51523(11) 0.0891(8) Uani 1 1 d . . . . .
H00P H 0.3255 0.7321 0.5135 0.107 Uiso 1 1 calc R . . . .
H00T H 0.2303 0.6762 0.5554 0.107 Uiso 1 1 calc R . . . .
C00U C 0.1306(3) 0.7999(2) 0.49906(11) 0.0882(8) Uani 1 1 d . . . . .
H00U H 0.0392 0.7655 0.4905 0.106 Uiso 1 1 calc R . . . .
H00V H 0.1321 0.8531 0.5325 0.106 Uiso 1 1 calc R . . . .
C00V C 0.2809(3) 0.5300(3) 0.20177(16) 0.1045(10) Uani 1 1 d . . . . .
H00W H 0.3068 0.4530 0.1934 0.125 Uiso 1 1 calc R . . . .
C00W C 0.2226(4) 0.2597(3) 0.33611(14) 0.0993(9) Uani 1 1 d . . . . .
H00X H 0.2058 0.1946 0.3109 0.119 Uiso 1 1 calc R . . . .
C00X C 0.3205(3) 0.6248(3) 0.17025(13) 0.0974(9) Uani 1 1 d . . . . .
H00Y H 0.3726 0.6112 0.1402 0.117 Uiso 1 1 calc R . . . .
C00Y C 0.3485(4) 0.3149(3) 0.34279(14) 0.1029(9) Uani 1 1 d . . . . .
H00Z H 0.4170 0.2869 0.3225 0.123 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O001 H001 0.8200 . ?
O001 C00C 1.334(3) . ?
O002 H002 0.8200 . ?
O002 C00H 1.347(3) . ?
O003 H003 0.8200 . ?
O003 C00A 1.347(3) . ?
N004 C009 1.261(3) . ?
N004 C00K 1.458(3) . ?
N005 C00N 1.468(3) . ?
N005 C00P 1.459(3) . ?
N005 C00U 1.469(3) . ?
N006 C00D 1.260(3) . ?
N006 C00T 1.452(3) . ?
N007 C00J 1.271(3) . ?
N007 C00O 1.444(3) . ?
C008 C009 1.460(3) . ?
C008 C00A 1.400(3) . ?
C008 C00E 1.384(3) . ?
C009 H009 0.9300 . ?
C00A C00I 1.386(3) . ?
C00B C00C 1.406(3) . ?
C00B C00D 1.457(3) . ?
C00B C00R 1.381(3) . ?
C00C C00M 1.390(4) . ?
C00D H00D 0.9300 . ?
C00E H00E 0.9300 . ?
C00E C00L 1.379(3) . ?
C00F H00F 0.9300 . ?
C00F C00I 1.355(3) . ?
C00F C00L 1.373(3) . ?
C00G C00H 1.410(3) . ?
C00G C00J 1.439(3) . ?
C00G C00S 1.391(4) . ?
C00H C00Q 1.376(3) . ?
C00I H00I 0.9300 . ?
C00J H00J 0.9300 . ?
C00K H00A 0.9700 . ?
C00K H00B 0.9700 . ?
C00K C00P 1.506(3) . ?
C00L H00L 0.9300 . ?
C00M H00M 0.9300 . ?
C00M C00W 1.358(4) . ?
C00N H00C 0.9700 . ?
C00N H00G 0.9700 . ?
C00N C00O 1.516(4) . ?
C00O H00H 0.9700 . ?
C00O H00K 0.9700 . ?
C00P H00N 0.9700 . ?
C00P H00O 0.9700 . ?
C00Q H00Q 0.9300 . ?
C00Q C00X 1.369(4) . ?
C00R H00R 0.9300 . ?
C00R C00Y 1.380(4) . ?
C00S H00S 0.9300 . ?
C00S C00V 1.373(4) . ?
C00T H00P 0.9700 . ?
C00T H00T 0.9700 . ?
C00T C00U 1.502(4) . ?
C00U H00U 0.9700 . ?
C00U H00V 0.9700 . ?
C00V H00W 0.9300 . ?
C00V C00X 1.374(5) . ?
C00W H00X 0.9300 . ?
C00W C00Y 1.371(4) . ?
C00X H00Y 0.9300 . ?
C00Y H00Z 0.9300 . ?

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
C00C O001 H001 109.5 . . ?
C00H O002 H002 109.5 . . ?
C00A O003 H003 109.5 . . ?
C009 N004 C00K 119.1(2) . . ?
C00N N005 C00U 111.8(2) . . ?
C00P N005 C00N 112.4(2) . . ?
C00P N005 C00U 112.0(2) . . ?
C00D N006 C00T 121.1(2) . . ?
C00J N007 C00O 119.8(2) . . ?
C00A C008 C009 121.48(19) . . ?
C00E C008 C009 120.61(18) . . ?
C00E C008 C00A 117.91(19) . . ?
N004 C009 C008 122.08(19) . . ?
N004 C009 H009 119.0 . . ?
C008 C009 H009 119.0 . . ?
O003 C00A C008 120.7(2) . . ?
O003 C00A C00I 119.34(19) . . ?
C00I C00A C008 119.9(2) . . ?
C00C C00B C00D 120.3(2) . . ?
C00R C00B C00C 118.6(2) . . ?
C00R C00B C00D 121.1(2) . . ?
O001 C00C C00B 121.5(2) . . ?
O001 C00C C00M 119.2(2) . . ?
C00M C00C C00B 119.3(2) . . ?
N006 C00D C00B 121.6(2) . . ?
N006 C00D H00D 119.2 . . ?
C00B C00D H00D 119.2 . . ?
C008 C00E H00E 119.2 . . ?
C00L C00E C008 121.6(2) . . ?
C00L C00E H00E 119.2 . . ?
C00I C00F H00F 119.7 . . ?
C00I C00F C00L 120.7(2) . . ?
C00L C00F H00F 119.7 . . ?
C00H C00G C00J 120.6(2) . . ?
C00S C00G C00H 118.2(3) . . ?
C00S C00G C00J 121.1(2) . . ?
O002 C00H C00G 121.2(2) . . ?
O002 C00H C00Q 118.9(2) . . ?
C00Q C00H C00G 119.9(3) . . ?
C00A C00I H00I 119.7 . . ?
C00F C00I C00A 120.6(2) . . ?
C00F C00I H00I 119.7 . . ?
N007 C00J C00G 122.2(2) . . ?
N007 C00J H00J 118.9 . . ?
C00G C00J H00J 118.9 . . ?
N004 C00K H00A 109.6 . . ?
N004 C00K H00B 109.6 . . ?
N004 C00K C00P 110.1(2) . . ?
H00A C00K H00B 108.2 . . ?
C00P C00K H00A 109.6 . . ?
C00P C00K H00B 109.6 . . ?
C00E C00L H00L 120.4 . . ?
C00F C00L C00E 119.2(2) . . ?
C00F C00L H00L 120.4 . . ?
C00C C00M H00M 119.6 . . ?
C00W C00M C00C 120.8(3) . . ?
C00W C00M H00M 119.6 . . ?
N005 C00N H00C 109.2 . . ?
N005 C00N H00G 109.2 . . ?
N005 C00N C00O 111.9(2) . . ?
H00C C00N H00G 107.9 . . ?
C00O C00N H00C 109.2 . . ?
C00O C00N H00G 109.2 . . ?
N007 C00O C00N 111.7(2) . . ?
N007 C00O H00H 109.3 . . ?
N007 C00O H00K 109.3 . . ?
C00N C00O H00H 109.3 . . ?
C00N C00O H00K 109.3 . . ?
H00H C00O H00K 107.9 . . ?
N005 C00P C00K 112.0(2) . . ?
N005 C00P H00N 109.2 . . ?
N005 C00P H00O 109.2 . . ?
C00K C00P H00N 109.2 . . ?
C00K C00P H00O 109.2 . . ?
H00N C00P H00O 107.9 . . ?
C00H C00Q H00Q 119.9 . . ?
C00X C00Q C00H 120.3(3) . . ?
C00X C00Q H00Q 119.9 . . ?
C00B C00R H00R 119.5 . . ?
C00Y C00R C00B 121.0(3) . . ?
C00Y C00R H00R 119.5 . . ?
C00G C00S H00S 119.5 . . ?
C00V C00S C00G 121.1(3) . . ?
C00V C00S H00S 119.5 . . ?
N006 C00T H00P 109.5 . . ?
N006 C00T H00T 109.5 . . ?
N006 C00T C00U 110.9(2) . . ?
H00P C00T H00T 108.0 . . ?
C00U C00T H00P 109.5 . . ?
C00U C00T H00T 109.5 . . ?
N005 C00U C00T 112.3(2) . . ?
N005 C00U H00U 109.1 . . ?
N005 C00U H00V 109.1 . . ?
C00T C00U H00U 109.1 . . ?
C00T C00U H00V 109.1 . . ?
H00U C00U H00V 107.9 . . ?
C00S C00V H00W 120.2 . . ?
C00S C00V C00X 119.6(3) . . ?
C00X C00V H00W 120.2 . . ?
C00M C00W H00X 119.8 . . ?
C00M C00W C00Y 120.5(3) . . ?
C00Y C00W H00X 119.8 . . ?
C00Q C00X C00V 120.9(3) . . ?
C00Q C00X H00Y 119.6 . . ?
C00V C00X H00Y 119.6 . . ?
C00R C00Y H00Z 120.1 . . ?
C00W C00Y C00R 119.8(3) . . ?
C00W C00Y H00Z 120.1 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-26
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zxg-zxh-4
_database_code_depnum_ccdc_archive 'CCDC 1504829'
_audit_update_record             
;
2016-09-18 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_audit_creation_date             2016-05-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C9 H9 F N1.33 O)'
_chemical_formula_sum            'C18 H18 F2 N2.67 O2'
_chemical_formula_weight         341.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   14.4761(5)
_cell_length_b                   14.4761(5)
_cell_length_c                   40.5191(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7353.4(6)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    3411
_cell_measurement_temperature    294.37(10)
_cell_measurement_theta_max      72.6270
_cell_measurement_theta_min      4.1490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76192
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            9115
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.712
_diffrn_reflns_theta_min         4.147
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.37(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   57.0000 -150.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega   32.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921 -139.0000 -134.0000 65

#__ type_ start__ end____ width___ exp.time_
  3 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -77.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega   38.00   91.00   1.0000    2.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

#__ type_ start__ end____ width___ exp.time_
  5 omega   38.00   91.00   1.0000    2.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00   91.00   1.0000    2.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
  7 omega   38.00   91.00   1.0000    2.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

#__ type_ start__ end____ width___ exp.time_
  8 omega   87.00  178.00   1.0000    2.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -150.0000 91

#__ type_ start__ end____ width___ exp.time_
  9 omega   91.00  176.00   1.0000    2.7200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 85

#__ type_ start__ end____ width___ exp.time_
 10 omega   10.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   77.0000  -30.0000 92

#__ type_ start__ end____ width___ exp.time_
 11 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   77.0000   90.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0372902000
_diffrn_orient_matrix_UB_12      0.0031294000
_diffrn_orient_matrix_UB_13      0.0353629000
_diffrn_orient_matrix_UB_21      -0.0155569000
_diffrn_orient_matrix_UB_22      0.0943505000
_diffrn_orient_matrix_UB_23      -0.0095952000
_diffrn_orient_matrix_UB_31      -0.1160628000
_diffrn_orient_matrix_UB_32      -0.0788041000
_diffrn_orient_matrix_UB_33      -0.0100682000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2682
_reflns_number_total             3188
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0681
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1140P)²+2.5190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1790
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C009(H00E,H00G), C00E(H00I,H00K), C00I(H00A,H00B), C00N(H00C,H00D)
2.b Aromatic/amide H refined with riding coordinates:
 C00B(H00H), C00F(H00F), C00J(H00J), C00L(H00L), C00M(H00M), C00O(H00O),
 C00P(H00P), C00Q(H00Q)
2.c Idealised tetrahedral OH refined as rotating group:
 O004(H004), O005(H005)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F001 F 1.09022(12) 0.68975(13) 0.42664(4) 0.0817(5) Uani 1 1 d . . . . .
N002 N 0.6667 0.3333 0.52714(6) 0.0397(5) Uani 1 3 d S T P . .
F003 F 0.64232(13) 0.69443(12) 0.41544(4) 0.0827(5) Uani 1 1 d . . . . .
O004 O 0.58399(14) 0.55228(12) 0.46541(3) 0.0628(4) Uani 1 1 d . . . . .
H004 H 0.5695 0.5030 0.4782 0.094 Uiso 1 1 calc GR . . . .
O005 O 1.00751(16) 0.73709(16) 0.37425(4) 0.0737(5) Uani 1 1 d . . . . .
H005 H 0.9759 0.7531 0.3606 0.111 Uiso 1 1 calc GR . . . .
N006 N 1.0000 1.0000 0.30979(6) 0.0485(6) Uani 1 3 d S T P . .
N007 N 0.51199(13) 0.35778(12) 0.48320(4) 0.0498(4) Uani 1 1 d . . . . .
N008 N 0.88703(14) 0.80318(13) 0.35284(4) 0.0557(4) Uani 1 1 d . . . . .
C009 C 0.56941(13) 0.33259(14) 0.53692(4) 0.0447(4) Uani 1 1 d . . . . .
H00E H 0.5859 0.4052 0.5413 0.054 Uiso 1 1 calc R . . . .
H00G H 0.5427 0.2922 0.5572 0.054 Uiso 1 1 calc R . . . .
C00A C 0.91781(15) 0.79843(14) 0.41008(4) 0.0481(4) Uani 1 1 d . . . . .
C00B C 0.51462(15) 0.33484(16) 0.45270(5) 0.0511(4) Uani 1 1 d . . . . .
H00H H 0.4949 0.2650 0.4471 0.061 Uiso 1 1 calc R . . . .
C00C C 0.54653(15) 0.41212(17) 0.42713(5) 0.0522(5) Uani 1 1 d . . . . .
C00D C 0.98423(15) 0.75476(15) 0.40435(5) 0.0512(4) Uani 1 1 d . . . . .
C00E C 0.48315(14) 0.28424(15) 0.51072(5) 0.0497(4) Uani 1 1 d . . . . .
H00I H 0.4754 0.2171 0.5032 0.060 Uiso 1 1 calc R . . . .
H00K H 0.4155 0.2702 0.5199 0.060 Uiso 1 1 calc R . . . .
C00F C 0.87174(15) 0.82353(15) 0.38226(5) 0.0513(4) Uani 1 1 d . . . . .
H00F H 0.8303 0.8551 0.3859 0.062 Uiso 1 1 calc R . . . .
C00G C 0.58031(15) 0.52011(16) 0.43568(5) 0.0515(5) Uani 1 1 d . . . . .
C00H C 1.02647(16) 0.73153(16) 0.43194(5) 0.0545(5) Uani 1 1 d . . . . .
C00I C 0.92958(18) 0.89005(17) 0.29942(4) 0.0587(5) Uani 1 1 d . . . . .
H00A H 0.9715 0.8554 0.2962 0.070 Uiso 1 1 calc R . . . .
H00B H 0.8973 0.8900 0.2784 0.070 Uiso 1 1 calc R . . . .
C00J C 1.00471(16) 0.74741(17) 0.46340(5) 0.0601(5) Uani 1 1 d . . . . .
H00J H 1.0336 0.7298 0.4812 0.072 Uiso 1 1 calc R . . . .
C00K C 0.61109(17) 0.59133(19) 0.40851(6) 0.0607(5) Uani 1 1 d . . . . .
C00L C 0.93911(18) 0.7902(2) 0.46867(5) 0.0653(6) Uani 1 1 d . . . . .
H00L H 0.9240 0.8017 0.4901 0.078 Uiso 1 1 calc R . . . .
C00M C 0.89657(17) 0.81551(18) 0.44247(5) 0.0598(5) Uani 1 1 d . . . . .
H00M H 0.8529 0.8445 0.4462 0.072 Uiso 1 1 calc R . . . .
C00N C 0.84259(17) 0.82720(18) 0.32425(5) 0.0625(5) Uani 1 1 d . . . . .
H00C H 0.8095 0.8682 0.3310 0.075 Uiso 1 1 calc R . . . .
H00D H 0.7882 0.7614 0.3143 0.075 Uiso 1 1 calc R . . . .
C00O C 0.5438(2) 0.3815(2) 0.39398(5) 0.0681(6) Uani 1 1 d . . . . .
H00O H 0.5203 0.3104 0.3890 0.082 Uiso 1 1 calc R . . . .
C00P C 0.60982(19) 0.5613(2) 0.37672(6) 0.0733(7) Uani 1 1 d . . . . .
H00P H 0.6321 0.6118 0.3599 0.088 Uiso 1 1 calc R . . . .
C00Q C 0.5751(2) 0.4549(3) 0.36917(6) 0.0784(7) Uani 1 1 d . . . . .
H00Q H 0.5734 0.4340 0.3474 0.094 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F001 C00H 1.350(2) . ?
N002 C009 1.4575(18) 2_655 ?
N002 C009 1.4575(18) 3_665 ?
N002 C009 1.4575(18) . ?
F003 C00K 1.355(3) . ?
O004 H004 0.8200 . ?
O004 C00G 1.283(2) . ?
O005 H005 0.8200 . ?
O005 C00D 1.324(2) . ?
N006 C00I 1.458(2) . ?
N006 C00I 1.458(2) 2_765 ?
N006 C00I 1.458(2) 3_675 ?
N007 C00B 1.285(2) . ?
N007 C00E 1.451(2) . ?
N008 C00F 1.274(2) . ?
N008 C00N 1.449(3) . ?
C009 H00E 0.9700 . ?
C009 H00G 0.9700 . ?
C009 C00E 1.517(2) . ?
C00A C00D 1.409(3) . ?
C00A C00F 1.446(3) . ?
C00A C00M 1.398(3) . ?
C00B H00H 0.9300 . ?
C00B C00C 1.422(3) . ?
C00C C00G 1.428(3) . ?
C00C C00O 1.409(3) . ?
C00D C00H 1.394(3) . ?
C00E H00I 0.9700 . ?
C00E H00K 0.9700 . ?
C00F H00F 0.9300 . ?
C00G C00K 1.419(3) . ?
C00H C00J 1.360(3) . ?
C00I H00A 0.9700 . ?
C00I H00B 0.9700 . ?
C00I C00N 1.510(3) . ?
C00J H00J 0.9300 . ?
C00J C00L 1.385(3) . ?
C00K C00P 1.356(3) . ?
C00L H00L 0.9300 . ?
C00L C00M 1.367(3) . ?
C00M H00M 0.9300 . ?
C00N H00C 0.9700 . ?
C00N H00D 0.9700 . ?
C00O H00O 0.9300 . ?
C00O C00Q 1.365(4) . ?
C00P H00P 0.9300 . ?
C00P C00Q 1.396(4) . ?
C00Q H00Q 0.9300 . ?

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
C009 N002 C009 112.90(9) 2_655 3_665 ?
C009 N002 C009 112.90(9) 3_665 . ?
C009 N002 C009 112.90(9) 2_655 . ?
C00G O004 H004 109.5 . . ?
C00D O005 H005 109.5 . . ?
C00I N006 C00I 112.05(10) 3_675 . ?
C00I N006 C00I 112.05(10) 2_765 . ?
C00I N006 C00I 112.05(10) 2_765 3_675 ?
C00B N007 C00E 125.74(16) . . ?
C00F N008 C00N 122.90(19) . . ?
N002 C009 H00E 109.1 . . ?
N002 C009 H00G 109.1 . . ?
N002 C009 C00E 112.47(15) . . ?
H00E C009 H00G 107.8 . . ?
C00E C009 H00E 109.1 . . ?
C00E C009 H00G 109.1 . . ?
C00D C00A C00F 119.23(17) . . ?
C00M C00A C00D 119.60(18) . . ?
C00M C00A C00F 121.17(17) . . ?
N007 C00B H00H 118.7 . . ?
N007 C00B C00C 122.50(18) . . ?
C00C C00B H00H 118.7 . . ?
C00B C00C C00G 118.92(17) . . ?
C00O C00C C00B 120.0(2) . . ?
C00O C00C C00G 121.1(2) . . ?
O005 C00D C00A 122.36(18) . . ?
O005 C00D C00H 120.51(18) . . ?
C00H C00D C00A 117.13(17) . . ?
N007 C00E C009 109.32(15) . . ?
N007 C00E H00I 109.8 . . ?
N007 C00E H00K 109.8 . . ?
C009 C00E H00I 109.8 . . ?
C009 C00E H00K 109.8 . . ?
H00I C00E H00K 108.3 . . ?
N008 C00F C00A 121.08(18) . . ?
N008 C00F H00F 119.5 . . ?
C00A C00F H00F 119.5 . . ?
O004 C00G C00C 123.67(18) . . ?
O004 C00G C00K 121.58(19) . . ?
C00K C00G C00C 114.75(19) . . ?
F001 C00H C00D 117.47(18) . . ?
F001 C00H C00J 119.53(19) . . ?
C00J C00H C00D 122.99(19) . . ?
N006 C00I H00A 109.1 . . ?
N006 C00I H00B 109.1 . . ?
N006 C00I C00N 112.51(17) . . ?
H00A C00I H00B 107.8 . . ?
C00N C00I H00A 109.1 . . ?
C00N C00I H00B 109.1 . . ?
C00H C00J H00J 120.4 . . ?
C00H C00J C00L 119.3(2) . . ?
C00L C00J H00J 120.4 . . ?
F003 C00K C00G 116.8(2) . . ?
F003 C00K C00P 119.5(2) . . ?
C00P C00K C00G 123.7(2) . . ?
C00J C00L H00L 119.9 . . ?
C00M C00L C00J 120.12(19) . . ?
C00M C00L H00L 119.9 . . ?
C00A C00M H00M 119.6 . . ?
C00L C00M C00A 120.90(19) . . ?
C00L C00M H00M 119.6 . . ?
N008 C00N C00I 109.91(18) . . ?
N008 C00N H00C 109.7 . . ?
N008 C00N H00D 109.7 . . ?
C00I C00N H00C 109.7 . . ?
C00I C00N H00D 109.7 . . ?
H00C C00N H00D 108.2 . . ?
C00C C00O H00O 119.6 . . ?
C00Q C00O C00C 120.7(2) . . ?
C00Q C00O H00O 119.6 . . ?
C00K C00P H00P 119.9 . . ?
C00K C00P C00Q 120.1(2) . . ?
C00Q C00P H00P 119.9 . . ?
C00O C00Q C00P 119.6(2) . . ?
C00O C00Q H00Q 120.2 . . ?
C00P C00Q H00Q 120.2 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-05-13
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zxg-zxh-2
_database_code_depnum_ccdc_archive 'CCDC 1504828'
_audit_update_record             
;
2016-09-18 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_audit_creation_date             2016-05-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H34 N4 O6'
_chemical_formula_sum            'C30 H34 N4 O6'
_chemical_formula_weight         546.61
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.29545(12)
_cell_length_b                   15.9502(4)
_cell_length_c                   28.8235(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2894.28(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3410
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.5750
_cell_measurement_theta_min      8.1560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28952
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            9429
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.517
_diffrn_reflns_theta_min         5.756
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   20.00  104.00   1.0000    3.5200
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega   20.00  104.00   1.0000    3.5200
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000   60.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega   23.00   90.00   1.0000    3.5200
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000   90.0000 67

#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   75.00   1.0000    3.5200
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  120.0000 74

#__ type_ start__ end____ width___ exp.time_
  5 omega   38.00   91.00   1.0000   14.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

#__ type_ start__ end____ width___ exp.time_
  6 omega   40.00   98.00   1.0000   14.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
  7 omega   38.00   91.00   1.0000   14.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
  8 omega   40.00   98.00   1.0000   14.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
  9 omega   39.00  109.00   1.0000   14.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 70

#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00   97.00   1.0000   14.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 57

#__ type_ start__ end____ width___ exp.time_
 11 omega   53.00   87.00   1.0000   14.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0715273000
_diffrn_orient_matrix_UB_12      -0.0852044000
_diffrn_orient_matrix_UB_13      0.0198593000
_diffrn_orient_matrix_UB_21      -0.0742730000
_diffrn_orient_matrix_UB_22      -0.0437927000
_diffrn_orient_matrix_UB_23      -0.0447718000
_diffrn_orient_matrix_UB_31      0.2219944000
_diffrn_orient_matrix_UB_32      0.0127700000
_diffrn_orient_matrix_UB_33      -0.0212766000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.652
_reflns_Friedel_fraction_full    0.911
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                4829
_reflns_number_total             5372
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Flack x determined using 1652 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(17)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0576
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1064P)²+0.0689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1640
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 C00O
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C00O: within 2A with sigma of 0.007 and sigma for terminal atoms of 0.001
4. Others
 Sof(C0)=Sof(H0)=1-FVAR(1)
 Sof(C013)=Sof(H013)=FVAR(1)
 Sof(C2A)=Sof(H2AA)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=FVAR(2)
 Sof(N1A)=1-FVAR(3)
 Sof(N1)=FVAR(3)
 Sof(C3A)=Sof(H3A)=1-FVAR(4)
 Sof(C3)=Sof(H2B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00B), C00M(H00C,H00D), C00O(H00E,H00H), C00P(H00I,H00L)
5.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00J(H00J), C00K(H00K), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00V(H00V), C00Y(H00Y), C00Z(H00Z), C013(H013), C0(H0),
  C2A(H2AA), C3A(H3A)
5.c Idealised Me refined as rotating group:
 C00U(H00M,H00N,H00O), C00X(H00P,H00U,H00W), C012(H01A,H01B,H01C)
5.d Idealised tetrahedral OH refined as rotating group:
 O001(H001), O002(H002), O009(H009)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O001 O 0.2053(4) 0.26138(14) 0.64107(10) 0.0640(6) Uani 1 1 d . . . . .
H001 H 0.3076 0.2657 0.6236 0.096 Uiso 1 1 calc GR . . . .
O002 O 1.3024(4) 0.56514(16) 0.65945(8) 0.0637(6) Uani 1 1 d . . . . .
H002 H 1.1963 0.5428 0.6485 0.096 Uiso 1 1 calc GR . . . .
O003 O 1.6453(4) 0.61799(18) 0.70076(9) 0.0720(7) Uani 1 1 d . . . . .
O004 O -0.1399(4) 0.23008(16) 0.68783(10) 0.0705(7) Uani 1 1 d . . . . .
N005 N 0.5085(4) 0.20946(18) 0.58863(9) 0.0577(6) Uani 1 1 d . . . . .
N006 N 0.9866(5) 0.46452(18) 0.65537(9) 0.0587(6) Uani 1 1 d . . . . .
N007 N 0.6428(4) 0.37870(18) 0.56166(12) 0.0643(7) Uani 1 1 d . . . . .
O008 O -0.1483(6) 0.6709(2) 0.38729(12) 0.0920(9) Uani 1 1 d . . . . .
O009 O 0.0655(7) 0.5747(2) 0.44400(15) 0.1062(13) Uani 1 1 d . . . . .
H009 H 0.1364 0.5516 0.4642 0.159 Uiso 1 1 calc GR . . . .
C00A C 1.3627(5) 0.52391(18) 0.69753(10) 0.0501(6) Uani 1 1 d . . . . .
C00B C 0.2432(5) 0.1171(2) 0.61786(10) 0.0554(7) Uani 1 1 d . . . . .
C00C C 0.1368(5) 0.18166(19) 0.64117(11) 0.0518(6) Uani 1 1 d . . . . .
C00D C 1.5482(5) 0.5509(2) 0.72051(11) 0.0571(7) Uani 1 1 d . . . . .
C00E C 1.2502(5) 0.45517(19) 0.71476(11) 0.0534(6) Uani 1 1 d . . . . .
C00F C 0.4353(6) 0.1360(2) 0.59155(11) 0.0575(7) Uani 1 1 d . . . . .
H00F H 0.5059 0.0927 0.5765 0.069 Uiso 1 1 calc R . . . .
C00G C 1.0587(6) 0.4273(2) 0.69129(12) 0.0584(7) Uani 1 1 d . . . . .
H00G H 0.9862 0.3810 0.7028 0.070 Uiso 1 1 calc R . . . .
C00H C -0.0492(5) 0.1632(2) 0.66623(12) 0.0571(7) Uani 1 1 d . . . . .
C00I C 0.0324(7) 0.7050(2) 0.40602(13) 0.0705(9) Uani 1 1 d . . . . .
C00J C 1.5013(7) 0.4430(3) 0.77731(13) 0.0741(10) Uani 1 1 d . . . . .
H00J H 1.5465 0.4164 0.8043 0.089 Uiso 1 1 calc R . . . .
C00K C -0.1281(6) 0.0825(2) 0.66675(13) 0.0660(8) Uani 1 1 d . . . . .
H00K H -0.2525 0.0704 0.6828 0.079 Uiso 1 1 calc R . . . .
C00L C 0.8369(5) 0.4086(2) 0.58426(13) 0.0632(8) Uani 1 1 d . . . . .
H00A H 0.8928 0.4563 0.5673 0.076 Uiso 1 1 calc R . . . .
H00B H 0.9432 0.3646 0.5838 0.076 Uiso 1 1 calc R . . . .
C00M C 0.7931(6) 0.4337(2) 0.63340(13) 0.0655(8) Uani 1 1 d . . . . .
H00C H 0.6854 0.4772 0.6339 0.079 Uiso 1 1 calc R . . . .
H00D H 0.7394 0.3858 0.6505 0.079 Uiso 1 1 calc R . . . .
C00N C 0.1444(8) 0.6515(2) 0.43581(14) 0.0727(10) Uani 1 1 d . . . . .
C00O C 0.6760(6) 0.3050(2) 0.53348(11) 0.0587(7) Uani 1 1 d . U . . .
H00E H 0.8027 0.3127 0.5148 0.070 Uiso 1 1 calc R . . . .
H00H H 0.5566 0.2983 0.5125 0.070 Uiso 1 1 calc R . . . .
C00P C 0.7000(6) 0.2262(2) 0.56235(13) 0.0642(8) Uani 1 1 d . . . . .
H00I H 0.7300 0.1791 0.5421 0.077 Uiso 1 1 calc R . . . .
H00L H 0.8187 0.2327 0.5835 0.077 Uiso 1 1 calc R . . . .
C00Q C 1.6150(6) 0.5105(2) 0.76003(13) 0.0662(8) Uani 1 1 d . . . . .
H00Q H 1.7369 0.5286 0.7752 0.079 Uiso 1 1 calc R . . . .
C00R C 0.1635(7) 0.0356(2) 0.61922(13) 0.0684(9) Uani 1 1 d . . . . .
H00R H 0.2348 -0.0074 0.6040 0.082 Uiso 1 1 calc R . . . .
C00S C 1.3226(7) 0.4150(2) 0.75491(13) 0.0680(9) Uani 1 1 d . . . . .
H00S H 1.2491 0.3689 0.7665 0.082 Uiso 1 1 calc R . . . .
C00T C -0.0198(8) 0.0190(2) 0.64298(16) 0.0770(10) Uani 1 1 d . . . . .
H00T H -0.0734 -0.0353 0.6434 0.092 Uiso 1 1 calc R . . . .
C00U C 1.8279(6) 0.6514(3) 0.72235(16) 0.0799(11) Uani 1 1 d . . . . .
H00M H 1.8807 0.6976 0.7044 0.120 Uiso 1 1 calc GR . . . .
H00N H 1.9353 0.6088 0.7244 0.120 Uiso 1 1 calc GR . . . .
H00O H 1.7921 0.6706 0.7529 0.120 Uiso 1 1 calc GR . . . .
C00V C 0.1101(9) 0.7839(3) 0.39763(16) 0.0849(12) Uani 1 1 d . . . . .
H00V H 0.0352 0.8196 0.3781 0.102 Uiso 1 1 calc R . . . .
C00W C 0.3350(9) 0.6792(3) 0.45550(15) 0.0817(11) Uani 1 1 d . . . . .
C00X C -0.3297(6) 0.2161(3) 0.71334(16) 0.0786(11) Uani 1 1 d . . . . .
H00P H -0.4351 0.1920 0.6933 0.118 Uiso 1 1 calc GR . . . .
H00U H -0.3809 0.2684 0.7254 0.118 Uiso 1 1 calc GR . . . .
H00W H -0.3013 0.1784 0.7386 0.118 Uiso 1 1 calc GR . . . .
C00Y C 0.2959(10) 0.8113(3) 0.4175(2) 0.0967(14) Uani 1 1 d . . . . .
H00Y H 0.3457 0.8650 0.4111 0.116 Uiso 1 1 calc R . . . .
C00Z C 0.4078(9) 0.7600(3) 0.44651(18) 0.0897(13) Uani 1 1 d . . . . .
H00Z H 0.5324 0.7791 0.4603 0.108 Uiso 1 1 calc R . . . .
C012 C -0.2566(10) 0.7189(4) 0.3534(2) 0.1040(17) Uani 1 1 d . . . . .
H01A H -0.1588 0.7353 0.3295 0.156 Uiso 1 1 calc GR . . . .
H01B H -0.3160 0.7680 0.3676 0.156 Uiso 1 1 calc GR . . . .
H01C H -0.3685 0.6859 0.3400 0.156 Uiso 1 1 calc GR . . . .
C013 C 0.490(2) 0.6189(5) 0.4768(4) 0.074(3) Uani 0.67(3) 1 d . . P A 1
H013 H 0.6248 0.6373 0.4850 0.089 Uiso 0.67(3) 1 calc R . P A 1
N1 N 0.4388(10) 0.5440(3) 0.4837(2) 0.068(2) Uani 0.610(14) 1 d . . P A 1
C2 C 0.5959(11) 0.4855(5) 0.5028(3) 0.074(2) Uani 0.609(12) 1 d . . P A 1
H2A H 0.7379 0.4948 0.4955 0.089 Uiso 0.609(12) 1 calc R . P A 1
C0 C 0.404(3) 0.6318(9) 0.4965(7) 0.063(5) Uani 0.33(3) 1 d . . P A 2
H0 H 0.5107 0.6556 0.5145 0.076 Uiso 0.33(3) 1 calc R . P A 2
C2A C 0.4481(19) 0.5117(7) 0.5452(4) 0.077(4) Uani 0.391(12) 1 d . . P A 2
H2AA H 0.4798 0.5427 0.5716 0.092 Uiso 0.391(12) 1 calc R . P A 2
N1A N 0.3318(16) 0.5615(6) 0.5094(4) 0.075(4) Uani 0.390(14) 1 d . . P A 2
C3 C 0.5675(18) 0.4441(7) 0.5199(5) 0.062(4) Uani 0.41(2) 1 d . . P A 1
H2B H 0.4315 0.4273 0.5115 0.075 Uiso 0.41(2) 1 calc R . P A 1
C3A C 0.5060(10) 0.4451(4) 0.5472(3) 0.056(3) Uani 0.59(2) 1 d . . P A 2
H3A H 0.4080 0.4170 0.5287 0.067 Uiso 0.59(2) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O001 H001 0.8200 . ?
O001 C00C 1.343(4) . ?
O002 H002 0.8200 . ?
O002 C00A 1.335(4) . ?
O003 C00D 1.358(4) . ?
O003 C00U 1.412(5) . ?
O004 C00H 1.360(4) . ?
O004 C00X 1.421(4) . ?
N005 C00F 1.261(4) . ?
N005 C00P 1.449(4) . ?
N006 C00G 1.277(5) . ?
N006 C00M 1.458(4) . ?
N007 C00L 1.464(4) . ?
N007 C00O 1.444(4) . ?
N007 C3 1.663(13) . ?
N007 C3A 1.427(6) . ?
O008 C00I 1.372(6) . ?
O008 C012 1.416(5) . ?
O009 H009 0.8200 . ?
O009 C00N 1.343(5) . ?
C00A C00D 1.410(4) . ?
C00A C00E 1.396(4) . ?
C00B C00C 1.400(4) . ?
C00B C00F 1.459(5) . ?
C00B C00R 1.395(5) . ?
C00C C00H 1.407(4) . ?
C00D C00Q 1.374(5) . ?
C00E C00G 1.452(5) . ?
C00E C00S 1.399(5) . ?
C00F H00F 0.9300 . ?
C00G H00G 0.9300 . ?
C00H C00K 1.380(5) . ?
C00I C00N 1.400(5) . ?
C00I C00V 1.372(7) . ?
C00J H00J 0.9300 . ?
C00J C00Q 1.386(6) . ?
C00J C00S 1.372(6) . ?
C00K H00K 0.9300 . ?
C00K C00T 1.400(6) . ?
C00L H00A 0.9700 . ?
C00L H00B 0.9700 . ?
C00L C00M 1.497(5) . ?
C00M H00C 0.9700 . ?
C00M H00D 0.9700 . ?
C00N C00W 1.399(7) . ?
C00O H00E 0.9700 . ?
C00O H00H 0.9700 . ?
C00O C00P 1.515(5) . ?
C00P H00I 0.9700 . ?
C00P H00L 0.9700 . ?
C00Q H00Q 0.9300 . ?
C00R H00R 0.9300 . ?
C00R C00T 1.367(6) . ?
C00S H00S 0.9300 . ?
C00T H00T 0.9300 . ?
C00U H00M 0.9600 . ?
C00U H00N 0.9600 . ?
C00U H00O 0.9600 . ?
C00V H00V 0.9300 . ?
C00V C00Y 1.374(8) . ?
C00W C00Z 1.393(6) . ?
C00W C013 1.500(9) . ?
C00W C0 1.468(14) . ?
C00X H00P 0.9600 . ?
C00X H00U 0.9600 . ?
C00X H00W 0.9600 . ?
C00Y H00Y 0.9300 . ?
C00Y C00Z 1.366(7) . ?
C00Z H00Z 0.9300 . ?
C012 H01A 0.9600 . ?
C012 H01B 0.9600 . ?
C012 H01C 0.9600 . ?
C013 H013 0.9300 . ?
C013 N1 1.253(9) . ?
N1 C2 1.468(9) . ?
C2 H2A 0.9300 . ?
C2 C3 0.842(14) . ?
C0 H0 0.9300 . ?
C0 N1A 1.267(17) . ?
C2A H2AA 0.9300 . ?
C2A N1A 1.492(12) . ?
C2A C3A 1.125(11) . ?
C3 H2B 0.9300 . ?
C3A H3A 0.9300 . ?

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
C00C O001 H001 109.5 . . ?
C00A O002 H002 109.5 . . ?
C00D O003 C00U 118.7(3) . . ?
C00H O004 C00X 117.8(3) . . ?
C00F N005 C00P 120.7(3) . . ?
C00G N006 C00M 119.5(3) . . ?
C00L N007 C3 110.8(4) . . ?
C00O N007 C00L 113.2(3) . . ?
C00O N007 C3 98.3(5) . . ?
C3A N007 C00L 113.1(3) . . ?
C3A N007 C00O 121.8(4) . . ?
C00I O008 C012 117.2(4) . . ?
C00N O009 H009 109.5 . . ?
O002 C00A C00D 118.1(3) . . ?
O002 C00A C00E 122.4(3) . . ?
C00E C00A C00D 119.5(3) . . ?
C00C C00B C00F 119.6(3) . . ?
C00R C00B C00C 120.0(3) . . ?
C00R C00B C00F 120.4(3) . . ?
O001 C00C C00B 122.8(3) . . ?
O001 C00C C00H 117.8(3) . . ?
C00B C00C C00H 119.4(3) . . ?
O003 C00D C00A 114.6(3) . . ?
O003 C00D C00Q 125.4(3) . . ?
C00Q C00D C00A 120.0(3) . . ?
C00A C00E C00G 119.7(3) . . ?
C00A C00E C00S 119.3(3) . . ?
C00S C00E C00G 121.0(3) . . ?
N005 C00F C00B 122.0(3) . . ?
N005 C00F H00F 119.0 . . ?
C00B C00F H00F 119.0 . . ?
N006 C00G C00E 122.1(3) . . ?
N006 C00G H00G 119.0 . . ?
C00E C00G H00G 119.0 . . ?
O004 C00H C00C 114.8(3) . . ?
O004 C00H C00K 125.1(3) . . ?
C00K C00H C00C 120.0(3) . . ?
O008 C00I C00N 114.7(4) . . ?
C00V C00I O008 126.1(4) . . ?
C00V C00I C00N 119.1(4) . . ?
C00Q C00J H00J 119.8 . . ?
C00S C00J H00J 119.8 . . ?
C00S C00J C00Q 120.5(3) . . ?
C00H C00K H00K 120.2 . . ?
C00H C00K C00T 119.6(3) . . ?
C00T C00K H00K 120.2 . . ?
N007 C00L H00A 109.5 . . ?
N007 C00L H00B 109.5 . . ?
N007 C00L C00M 110.8(3) . . ?
H00A C00L H00B 108.1 . . ?
C00M C00L H00A 109.5 . . ?
C00M C00L H00B 109.5 . . ?
N006 C00M C00L 110.3(3) . . ?
N006 C00M H00C 109.6 . . ?
N006 C00M H00D 109.6 . . ?
C00L C00M H00C 109.6 . . ?
C00L C00M H00D 109.6 . . ?
H00C C00M H00D 108.1 . . ?
O009 C00N C00I 118.5(4) . . ?
O009 C00N C00W 122.3(3) . . ?
C00W C00N C00I 119.2(4) . . ?
N007 C00O H00E 109.1 . . ?
N007 C00O H00H 109.1 . . ?
N007 C00O C00P 112.4(3) . . ?
H00E C00O H00H 107.9 . . ?
C00P C00O H00E 109.1 . . ?
C00P C00O H00H 109.1 . . ?
N005 C00P C00O 110.9(3) . . ?
N005 C00P H00I 109.5 . . ?
N005 C00P H00L 109.5 . . ?
C00O C00P H00I 109.5 . . ?
C00O C00P H00L 109.5 . . ?
H00I C00P H00L 108.0 . . ?
C00D C00Q C00J 120.3(3) . . ?
C00D C00Q H00Q 119.9 . . ?
C00J C00Q H00Q 119.9 . . ?
C00B C00R H00R 120.1 . . ?
C00T C00R C00B 119.9(4) . . ?
C00T C00R H00R 120.1 . . ?
C00E C00S H00S 119.8 . . ?
C00J C00S C00E 120.5(4) . . ?
C00J C00S H00S 119.8 . . ?
C00K C00T H00T 119.5 . . ?
C00R C00T C00K 121.1(3) . . ?
C00R C00T H00T 119.5 . . ?
O003 C00U H00M 109.5 . . ?
O003 C00U H00N 109.5 . . ?
O003 C00U H00O 109.5 . . ?
H00M C00U H00N 109.5 . . ?
H00M C00U H00O 109.5 . . ?
H00N C00U H00O 109.5 . . ?
C00I C00V H00V 119.2 . . ?
C00I C00V C00Y 121.5(4) . . ?
C00Y C00V H00V 119.2 . . ?
C00N C00W C013 121.4(4) . . ?
C00N C00W C0 114.7(7) . . ?
C00Z C00W C00N 119.9(4) . . ?
C00Z C00W C013 117.1(5) . . ?
C00Z C00W C0 121.9(7) . . ?
O004 C00X H00P 109.5 . . ?
O004 C00X H00U 109.5 . . ?
O004 C00X H00W 109.5 . . ?
H00P C00X H00U 109.5 . . ?
H00P C00X H00W 109.5 . . ?
H00U C00X H00W 109.5 . . ?
C00V C00Y H00Y 119.9 . . ?
C00Z C00Y C00V 120.2(5) . . ?
C00Z C00Y H00Y 119.9 . . ?
C00W C00Z H00Z 120.1 . . ?
C00Y C00Z C00W 119.9(5) . . ?
C00Y C00Z H00Z 120.1 . . ?
O008 C012 H01A 109.5 . . ?
O008 C012 H01B 109.5 . . ?
O008 C012 H01C 109.5 . . ?
H01A C012 H01B 109.5 . . ?
H01A C012 H01C 109.5 . . ?
H01B C012 H01C 109.5 . . ?
C00W C013 H013 119.7 . . ?
N1 C013 C00W 120.6(7) . . ?
N1 C013 H013 119.7 . . ?
C013 N1 C2 119.6(7) . . ?
N1 C2 H2A 117.5 . . ?
C3 C2 N1 125.1(11) . . ?
C3 C2 H2A 117.5 . . ?
C00W C0 H0 117.0 . . ?
N1A C0 C00W 125.9(10) . . ?
N1A C0 H0 117.0 . . ?
N1A C2A H2AA 112.9 . . ?
C3A C2A H2AA 112.9 . . ?
C3A C2A N1A 134.1(10) . . ?
C0 N1A C2A 119.9(10) . . ?
N007 C3 H2B 105.7 . . ?
C2 C3 N007 148.7(11) . . ?
C2 C3 H2B 105.7 . . ?
N007 C3A H3A 102.2 . . ?
C2A C3A N007 155.7(8) . . ?
C2A C3A H3A 102.2 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-05-06
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zxg-zxh
_database_code_depnum_ccdc_archive 'CCDC 1504827'
_audit_update_record             
;
2016-09-18 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_audit_creation_date             2016-09-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C39 H54 N4 O3)'
_chemical_formula_sum            'C78 H108 N8 O6'
_chemical_formula_weight         1253.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.9272(4)
_cell_length_b                   13.0256(4)
_cell_length_c                   23.4928(6)
_cell_angle_alpha                82.005(2)
_cell_angle_beta                 79.707(2)
_cell_angle_gamma                86.311(2)
_cell_volume                     3851.16(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.1550
_cell_measurement_theta_min      4.7570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55727
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42357
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.330
_diffrn_reflns_theta_min         4.755
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   23.00   89.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421 -125.0000 -150.0000 66

#__ type_ start__ end____ width___ exp.time_
  2 omega   17.00  105.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   38.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
  3 omega   19.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   19.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega   14.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   69.0000  -87.0000 89

#__ type_ start__ end____ width___ exp.time_
  6 omega  -33.00   55.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -38.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
  7 omega    1.00   75.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -99.0000   60.0000 74

#__ type_ start__ end____ width___ exp.time_
  8 omega    1.00   75.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -99.0000  -90.0000 74

#__ type_ start__ end____ width___ exp.time_
  9 omega   19.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   57.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
 10 omega    9.00  104.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 11 omega   40.00   98.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
 12 omega   40.00   98.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
 13 omega   39.00  109.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 70

#__ type_ start__ end____ width___ exp.time_
 14 omega   38.00   91.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 15 omega   40.00   65.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -60.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0976428000
_diffrn_orient_matrix_UB_12      -0.0084262000
_diffrn_orient_matrix_UB_13      -0.0477345000
_diffrn_orient_matrix_UB_21      -0.0518189000
_diffrn_orient_matrix_UB_22      -0.0849889000
_diffrn_orient_matrix_UB_23      -0.0235242000
_diffrn_orient_matrix_UB_31      -0.0497850000
_diffrn_orient_matrix_UB_32      0.0834573000
_diffrn_orient_matrix_UB_33      -0.0410333000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11557
_reflns_number_total             14910
_reflns_odcompleteness_completeness 61.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         14910
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0752
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1430P)²+0.6100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2383
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 N009, C00Q
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C00F, C00N
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C00Q(H00A,H00B), C00R(H00C,H00D), C00Z(H00E,H00G), C010(H01A,H01B), C014(H01M,
 H01N), C019(H01C,H01D), C01A(H01O,H01P), C01D(H01R,H01S), C01E(H01G,H01H),
 C01J(H01T,H01U), C01O(H01X,H01Y), C01U(H0AA,H)
3.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00K(H00K), C00M(H00M), C00O(H00O), C00S(H00S), C00V(H00V),
 C012(H012), C017(H017), C01B(H01E), C01C(H01F), C01F(H01I), C01G(H01J),
 C01H(H01K), C01K(H01W), C01L(H01L), C01Q(H01Q), C01R(H01Z), C01S(H01),
 C01V(H01V), C01W(H1AA), C01X(H2AA), C01Z(H3AA), C025(H025), C028(H028)
3.c Idealised Me refined as rotating group:
 C020(H02Z,HA,HB), C021(H02A,H02B,H02C), C022(H02D,H02E,H02F), C024(H02,HC,HD),
  C026(H4AA,HE,HF), C027(H5AA,HG,HH), C029(H02G,H02H,H02I), C02A(H6AA,HI,HJ),
 C02B(H7AA,HK,HL), C02C(H8AA,HM,HN), C02D(H02J,H02K,H02L), C02E(H9AA,HO,HP),
 C02F(H02M,H02N,H02O), C02G(H02P,H02Q,H02R), C02H(H02S,H02T,H02U), C02I(H02V,
 H02W,H02X), C02J(H0BA,HQ,HR), C02K(H02Y,HS,HT)
3.d Idealised tetrahedral OH refined as rotating group:
 O001(H001), O002(H002), O003(H003), O004(H004), O006(H006), O007(H007)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O001 O -0.22768(14) 0.39555(13) 0.88550(7) 0.0744(4) Uani 1 1 d . . . . .
H001 H -0.2364 0.3421 0.8725 0.112 Uiso 1 1 calc GR . . . .
O002 O 0.21705(13) 0.12234(12) 0.92916(9) 0.0761(5) Uani 1 1 d . . . . .
H002 H 0.1568 0.1027 0.9333 0.114 Uiso 1 1 calc GR . . . .
O003 O 0.63701(12) 1.01658(13) 0.61123(7) 0.0711(4) Uani 1 1 d . . . . .
H003 H 0.5736 1.0305 0.6147 0.107 Uiso 1 1 calc GR . . . .
O004 O 0.07936(15) 0.17705(13) 0.65662(7) 0.0749(4) Uani 1 1 d . . . . .
H004 H 0.0662 0.1302 0.6837 0.112 Uiso 1 1 calc GR . . . .
N005 N -0.10038(13) 0.04038(13) 0.85759(7) 0.0567(4) Uani 1 1 d . . . . .
O006 O 0.24213(15) 0.76505(15) 0.79477(8) 0.0833(5) Uani 1 1 d . . . . .
H006 H 0.2306 0.7624 0.7618 0.125 Uiso 1 1 calc GR . . . .
O007 O 0.53718(16) 0.53738(13) 0.57275(9) 0.0816(5) Uani 1 1 d . . . . .
H007 H 0.5193 0.5937 0.5563 0.122 Uiso 1 1 calc GR . . . .
N008 N 0.32152(13) 0.87119(13) 0.58766(8) 0.0588(4) Uani 1 1 d . . . . .
N009 N 0.01610(14) 0.13437(14) 0.93939(7) 0.0600(4) Uani 1 1 d . U . . .
N00A N 0.08657(15) 0.06689(15) 0.75634(8) 0.0669(5) Uani 1 1 d . . . . .
N00B N -0.19763(16) 0.25346(15) 0.81716(9) 0.0682(5) Uani 1 1 d . . . . .
N00C N 0.52048(15) 0.73845(15) 0.54778(9) 0.0683(5) Uani 1 1 d . . . . .
N00D N 0.26201(18) 0.70929(17) 0.69311(9) 0.0771(5) Uani 1 1 d . . . . .
N00E N 0.44074(15) 0.99929(17) 0.65127(10) 0.0751(5) Uani 1 1 d . . . . .
C00F C 0.02279(17) 0.23041(16) 0.92071(9) 0.0576(4) Uani 1 1 d . U . . .
H00F H -0.0385 0.2698 0.9163 0.069 Uiso 1 1 calc R . . . .
C00G C -0.15476(16) 0.45191(17) 0.84747(9) 0.0591(5) Uani 1 1 d . . . . .
C00H C 0.21800(17) 0.22536(16) 0.91113(9) 0.0601(5) Uani 1 1 d . . . . .
C00I C 0.13358(16) 0.24991(16) 0.67316(9) 0.0596(5) Uani 1 1 d . . . . .
C00J C -0.13009(17) 0.54891(17) 0.86007(10) 0.0632(5) Uani 1 1 d . . . . .
C00K C 0.58336(17) 0.74380(16) 0.58254(10) 0.0630(5) Uani 1 1 d . . . . .
H00K H 0.6021 0.8090 0.5880 0.076 Uiso 1 1 calc R . . . .
C00L C -0.10491(16) 0.41147(18) 0.79684(9) 0.0628(5) Uani 1 1 d . . . . .
C00M C 0.34783(19) 0.66089(17) 0.70207(10) 0.0670(5) Uani 1 1 d . . . . .
H00M H 0.3884 0.6291 0.6721 0.080 Uiso 1 1 calc R . . . .
C00N C 0.12304(17) 0.28116(16) 0.90593(9) 0.0571(4) Uani 1 1 d . U . . .
C00O C 0.13611(18) 0.13933(19) 0.76884(10) 0.0660(5) Uani 1 1 d . . . . .
H00O H 0.1565 0.1322 0.8052 0.079 Uiso 1 1 calc R . . . .
C00P C 0.16249(17) 0.23348(18) 0.72849(9) 0.0619(5) Uani 1 1 d . . . . .
C00Q C -0.08674(18) 0.08873(18) 0.95370(9) 0.0643(5) Uani 1 1 d . U . . .
H00A H -0.1406 0.1417 0.9461 0.077 Uiso 1 1 calc R . . . .
H00B H -0.1007 0.0622 0.9949 0.077 Uiso 1 1 calc R . . . .
C00R C -0.09143(18) 0.00167(17) 0.91812(9) 0.0630(5) Uani 1 1 d . . . . .
H00C H -0.0284 -0.0428 0.9187 0.076 Uiso 1 1 calc R . . . .
H00D H -0.1514 -0.0398 0.9357 0.076 Uiso 1 1 calc R . . . .
C00S C -0.12854(18) 0.30996(19) 0.78437(10) 0.0667(5) Uani 1 1 d . . . . .
H00S H -0.0914 0.2854 0.7509 0.080 Uiso 1 1 calc R . . . .
C00T C 0.32890(18) 0.70582(16) 0.80330(10) 0.0650(5) Uani 1 1 d . . . . .
C00U C 0.65845(18) 0.95957(16) 0.66055(10) 0.0616(5) Uani 1 1 d . . . . .
C00V C 0.1232(2) 0.38715(17) 0.88575(10) 0.0666(5) Uani 1 1 d . . . . .
H00V H 0.0604 0.4243 0.8820 0.080 Uiso 1 1 calc R . . . .
C00W C 0.62801(18) 0.65264(17) 0.61451(10) 0.0651(5) Uani 1 1 d . . . . .
C00X C 0.60341(17) 0.55185(17) 0.60887(10) 0.0619(5) Uani 1 1 d . . . . .
C00Y C 0.38434(19) 0.65372(16) 0.75760(10) 0.0662(5) Uani 1 1 d . . . . .
C00Z C -0.0543(2) -0.03316(16) 0.81778(11) 0.0701(6) Uani 1 1 d . . . . .
H00E H -0.0875 -0.0216 0.7834 0.084 Uiso 1 1 calc R . . . .
H00G H -0.0688 -0.1031 0.8367 0.084 Uiso 1 1 calc R . . . .
C010 C -0.20895(18) 0.06790(19) 0.85149(11) 0.0683(5) Uani 1 1 d . . . . .
H01A H -0.2463 0.0902 0.8876 0.082 Uiso 1 1 calc R . . . .
H01B H -0.2422 0.0069 0.8450 0.082 Uiso 1 1 calc R . . . .
C011 C 0.16090(19) 0.34026(18) 0.63448(10) 0.0671(5) Uani 1 1 d . . . . .
C012 C 0.46514(19) 0.9452(2) 0.69634(11) 0.0723(6) Uani 1 1 d . . . . .
H012 H 0.4117 0.9180 0.7254 0.087 Uiso 1 1 calc R . . . .
C013 C 0.31506(19) 0.27475(19) 0.89677(12) 0.0712(6) Uani 1 1 d . . . . .
C014 C 0.48033(19) 0.83288(19) 0.51728(10) 0.0716(6) Uani 1 1 d . . . . .
H01M H 0.5033 0.8333 0.4756 0.086 Uiso 1 1 calc R . . . .
H01N H 0.5095 0.8921 0.5287 0.086 Uiso 1 1 calc R . . . .
C015 C 0.36276(19) 0.69725(17) 0.85732(10) 0.0663(5) Uani 1 1 d . . . . .
C016 C 0.76353(19) 0.93496(17) 0.66673(11) 0.0683(5) Uani 1 1 d . . . . .
C017 C 0.4749(2) 0.59392(18) 0.76546(11) 0.0738(6) Uani 1 1 d . . . . .
H017 H 0.5119 0.5598 0.7354 0.089 Uiso 1 1 calc R . . . .
C018 C -0.1791(2) 0.59025(19) 0.91738(11) 0.0720(6) Uani 1 1 d . . . . .
C019 C 0.0632(2) -0.02415(19) 0.79915(12) 0.0773(6) Uani 1 1 d . . . . .
H01C H 0.0952 -0.0191 0.8329 0.093 Uiso 1 1 calc R . . . .
H01D H 0.0929 -0.0859 0.7825 0.093 Uiso 1 1 calc R . . . .
C01A C 0.3144(2) 0.98318(19) 0.58803(13) 0.0764(6) Uani 1 1 d . . . . .
H01O H 0.2455 1.0092 0.5805 0.092 Uiso 1 1 calc R . . . .
H01P H 0.3663 1.0147 0.5565 0.092 Uiso 1 1 calc R . . . .
C01B C 0.3096(2) 0.3802(2) 0.87778(12) 0.0782(7) Uani 1 1 d . . . . .
H01E H 0.3720 0.4153 0.8687 0.094 Uiso 1 1 calc R . . . .
C01C C 0.2172(2) 0.43609(18) 0.87148(11) 0.0751(6) Uani 1 1 d . . . . .
H01F H 0.2184 0.5065 0.8577 0.090 Uiso 1 1 calc R . . . .
C01D C 0.3622(2) 0.8433(2) 0.53004(10) 0.0725(6) Uani 1 1 d . . . . .
H01R H 0.3384 0.8957 0.5011 0.087 Uiso 1 1 calc R . . . .
H01S H 0.3335 0.7780 0.5264 0.087 Uiso 1 1 calc R . . . .
C01E C -0.2186(2) 0.1532(2) 0.80177(12) 0.0767(6) Uani 1 1 d . . . . .
H01G H -0.1691 0.1385 0.7674 0.092 Uiso 1 1 calc R . . . .
H01H H -0.2890 0.1553 0.7925 0.092 Uiso 1 1 calc R . . . .
C01F C -0.0548(2) 0.6026(2) 0.81931(12) 0.0780(6) Uani 1 1 d . . . . .
H01I H -0.0368 0.6673 0.8260 0.094 Uiso 1 1 calc R . . . .
C01G C 0.2174(2) 0.3081(2) 0.74613(12) 0.0791(7) Uani 1 1 d . . . . .
H01J H 0.2371 0.2971 0.7828 0.095 Uiso 1 1 calc R . . . .
C01H C -0.0296(2) 0.4691(2) 0.75788(11) 0.0781(7) Uani 1 1 d . . . . .
H01K H 0.0042 0.4431 0.7242 0.094 Uiso 1 1 calc R . . . .
C01I C 0.5746(2) 0.92381(19) 0.70431(11) 0.0721(6) Uani 1 1 d . . . . .
C01J C 0.33118(19) 1.0161(2) 0.64379(14) 0.0826(7) Uani 1 1 d . . . . .
H01T H 0.3110 1.0891 0.6441 0.099 Uiso 1 1 calc R . . . .
H01U H 0.2867 0.9771 0.6762 0.099 Uiso 1 1 calc R . . . .
C01K C 0.4534(2) 0.63674(19) 0.86271(12) 0.0758(6) Uani 1 1 d . . . . .
H01W H 0.4781 0.6299 0.8979 0.091 Uiso 1 1 calc R . . . .
C01L C 0.2149(2) 0.4118(2) 0.65516(13) 0.0818(7) Uani 1 1 d . . . . .
H01L H 0.2336 0.4728 0.6309 0.098 Uiso 1 1 calc R . . . .
C01M C 0.64587(19) 0.46465(18) 0.64116(11) 0.0674(5) Uani 1 1 d . . . . .
C01N C 0.85627(19) 0.9677(2) 0.61740(13) 0.0765(6) Uani 1 1 d . . . . .
C01O C 0.21993(18) 0.8261(2) 0.61003(12) 0.0759(6) Uani 1 1 d . . . . .
H01X H 0.1805 0.8294 0.5783 0.091 Uiso 1 1 calc R . . . .
H01Y H 0.1808 0.8670 0.6388 0.091 Uiso 1 1 calc R . . . .
C01P C 0.3053(2) 0.7554(2) 0.90688(11) 0.0782(6) Uani 1 1 d . . . . .
C01Q C -0.0055(2) 0.5635(3) 0.76912(13) 0.0925(8) Uani 1 1 d . . . . .
H01Q H 0.0445 0.6021 0.7429 0.111 Uiso 1 1 calc R . . . .
C01R C 0.5095(2) 0.5856(2) 0.81771(13) 0.0829(7) Uani 1 1 d . . . . .
H01Z H 0.5702 0.5459 0.8232 0.099 Uiso 1 1 calc R . . . .
C01S C 0.6971(2) 0.6668(2) 0.65149(14) 0.0841(7) Uani 1 1 d . . . . .
H01 H 0.7142 0.7335 0.6552 0.101 Uiso 1 1 calc R . . . .
C01T C 0.6175(2) 0.35420(19) 0.63709(13) 0.0789(7) Uani 1 1 d . . . . .
C01U C 0.2289(2) 0.7153(2) 0.63739(12) 0.0810(7) Uani 1 1 d . . . . .
H0AA H 0.1614 0.6838 0.6424 0.097 Uiso 1 1 calc R . . . .
H H 0.2795 0.6769 0.6118 0.097 Uiso 1 1 calc R . . . .
C01V C 0.2425(2) 0.3971(2) 0.71015(14) 0.0896(8) Uani 1 1 d . . . . .
H01V H 0.2779 0.4478 0.7223 0.108 Uiso 1 1 calc R . . . .
C01W C 0.5950(3) 0.8647(2) 0.75541(12) 0.0913(8) Uani 1 1 d . . . . .
H1AA H 0.5398 0.8413 0.7845 0.110 Uiso 1 1 calc R . . . .
C01X C 0.7790(3) 0.8758(2) 0.71872(14) 0.0881(8) Uani 1 1 d . . . . .
H2AA H 0.8477 0.8585 0.7244 0.106 Uiso 1 1 calc R . . . .
C01Y C 0.1312(3) 0.3580(2) 0.57354(12) 0.0908(8) Uani 1 1 d . . . . .
C01Z C 0.7141(2) 0.4842(2) 0.67677(13) 0.0836(7) Uani 1 1 d . . . . .
H3AA H 0.7441 0.4281 0.6980 0.100 Uiso 1 1 calc R . . . .
C020 C 0.1880(2) 0.7283(3) 0.92123(13) 0.0919(8) Uani 1 1 d . . . . .
H02Z H 0.1551 0.7514 0.8879 0.138 Uiso 1 1 calc GR . . . .
HA H 0.1536 0.7620 0.9537 0.138 Uiso 1 1 calc GR . . . .
HB H 0.1827 0.6545 0.9309 0.138 Uiso 1 1 calc GR . . . .
C021 C -0.1465(3) 0.5162(3) 0.96826(12) 0.1023(10) Uani 1 1 d . . . . .
H02A H -0.1734 0.4490 0.9688 0.153 Uiso 1 1 calc GR . . . .
H02B H -0.1747 0.5426 1.0043 0.153 Uiso 1 1 calc GR . . . .
H02C H -0.0712 0.5107 0.9636 0.153 Uiso 1 1 calc GR . . . .
C022 C -0.2996(2) 0.5986(3) 0.92368(16) 0.1000(9) Uani 1 1 d . . . . .
H02D H -0.3194 0.6480 0.8928 0.150 Uiso 1 1 calc GR . . . .
H02E H -0.3292 0.6209 0.9606 0.150 Uiso 1 1 calc GR . . . .
H02F H -0.3255 0.5320 0.9216 0.150 Uiso 1 1 calc GR . . . .
C023 C 0.4196(2) 0.2138(3) 0.90105(18) 0.0993(10) Uani 1 1 d . . . . .
C024 C 0.6689(3) 0.2743(2) 0.67885(16) 0.1043(10) Uani 1 1 d . . . . .
H02 H 0.7439 0.2801 0.6702 0.156 Uiso 1 1 calc GR . . . .
HC H 0.6514 0.2058 0.6742 0.156 Uiso 1 1 calc GR . . . .
HD H 0.6436 0.2870 0.7183 0.156 Uiso 1 1 calc GR . . . .
C025 C 0.7402(3) 0.5830(2) 0.68250(16) 0.0976(9) Uani 1 1 d . . . . .
H025 H 0.7866 0.5926 0.7072 0.117 Uiso 1 1 calc R . . . .
C026 C 0.8457(3) 0.9198(3) 0.56269(16) 0.1042(10) Uani 1 1 d . . . . .
H4AA H 0.8523 0.8456 0.5706 0.156 Uiso 1 1 calc GR . . . .
HE H 0.9000 0.9442 0.5311 0.156 Uiso 1 1 calc GR . . . .
HF H 0.7781 0.9396 0.5522 0.156 Uiso 1 1 calc GR . . . .
C027 C 0.8561(2) 1.0856(2) 0.60363(18) 0.1037(10) Uani 1 1 d . . . . .
H5AA H 0.7915 1.1107 0.5909 0.156 Uiso 1 1 calc GR . . . .
HG H 0.9143 1.1052 0.5733 0.156 Uiso 1 1 calc GR . . . .
HH H 0.8625 1.1152 0.6380 0.156 Uiso 1 1 calc GR . . . .
C028 C 0.6973(3) 0.8411(3) 0.76267(15) 0.1051(11) Uani 1 1 d . . . . .
H028 H 0.7118 0.8022 0.7968 0.126 Uiso 1 1 calc R . . . .
C029 C -0.1437(3) 0.6980(3) 0.92089(17) 0.1081(10) Uani 1 1 d . . . . .
H02G H -0.0692 0.6953 0.9205 0.162 Uiso 1 1 calc GR . . . .
H02H H -0.1797 0.7219 0.9563 0.162 Uiso 1 1 calc GR . . . .
H02I H -0.1599 0.7449 0.8881 0.162 Uiso 1 1 calc GR . . . .
C02A C 0.6627(4) 0.3290(2) 0.57482(15) 0.1149(13) Uani 1 1 d . . . . .
H6AA H 0.6278 0.3730 0.5471 0.172 Uiso 1 1 calc GR . . . .
HI H 0.6515 0.2578 0.5724 0.172 Uiso 1 1 calc GR . . . .
HJ H 0.7367 0.3407 0.5663 0.172 Uiso 1 1 calc GR . . . .
C02B C 0.3128(3) 0.8723(2) 0.88854(18) 0.1094(11) Uani 1 1 d . . . . .
H7AA H 0.3854 0.8900 0.8800 0.164 Uiso 1 1 calc GR . . . .
HK H 0.2765 0.9085 0.9197 0.164 Uiso 1 1 calc GR . . . .
HL H 0.2813 0.8920 0.8544 0.164 Uiso 1 1 calc GR . . . .
C02C C 0.3513(3) 0.7266(3) 0.96275(14) 0.1122(11) Uani 1 1 d . . . . .
H8AA H 0.3475 0.6532 0.9746 0.168 Uiso 1 1 calc GR . . . .
HM H 0.3119 0.7629 0.9930 0.168 Uiso 1 1 calc GR . . . .
HN H 0.4234 0.7456 0.9558 0.168 Uiso 1 1 calc GR . . . .
C02D C 0.4182(3) 0.1547(4) 0.9628(2) 0.1318(15) Uani 1 1 d . . . . .
H02J H 0.4025 0.2026 0.9910 0.198 Uiso 1 1 calc GR . . . .
H02K H 0.4859 0.1210 0.9652 0.198 Uiso 1 1 calc GR . . . .
H02L H 0.3655 0.1036 0.9705 0.198 Uiso 1 1 calc GR . . . .
C02E C 0.9626(3) 0.9329(3) 0.6343(2) 0.1175(12) Uani 1 1 d . . . . .
H9AA H 0.9709 0.9636 0.6680 0.176 Uiso 1 1 calc GR . . . .
HO H 1.0176 0.9545 0.6024 0.176 Uiso 1 1 calc GR . . . .
HP H 0.9663 0.8587 0.6431 0.176 Uiso 1 1 calc GR . . . .
C02F C 0.1820(4) 0.2707(3) 0.53884(14) 0.1317(16) Uani 1 1 d . . . . .
H02M H 0.2559 0.2642 0.5403 0.198 Uiso 1 1 calc GR . . . .
H02N H 0.1722 0.2869 0.4990 0.198 Uiso 1 1 calc GR . . . .
H02O H 0.1498 0.2065 0.5555 0.198 Uiso 1 1 calc GR . . . .
C02G C 0.1744(4) 0.4605(3) 0.53902(18) 0.1345(15) Uani 1 1 d . . . . .
H02P H 0.1441 0.5176 0.5590 0.202 Uiso 1 1 calc GR . . . .
H02Q H 0.1563 0.4689 0.5007 0.202 Uiso 1 1 calc GR . . . .
H02R H 0.2495 0.4587 0.5359 0.202 Uiso 1 1 calc GR . . . .
C02H C 0.0117(3) 0.3637(3) 0.57853(19) 0.1221(13) Uani 1 1 d . . . . .
H02S H -0.0173 0.3042 0.6037 0.183 Uiso 1 1 calc GR . . . .
H02T H -0.0065 0.3650 0.5406 0.183 Uiso 1 1 calc GR . . . .
H02U H -0.0163 0.4257 0.5945 0.183 Uiso 1 1 calc GR . . . .
C02I C 0.4380(3) 0.1385(3) 0.8542(2) 0.1266(15) Uani 1 1 d . . . . .
H02V H 0.3769 0.0984 0.8579 0.190 Uiso 1 1 calc GR . . . .
H02W H 0.4979 0.0929 0.8596 0.190 Uiso 1 1 calc GR . . . .
H02X H 0.4508 0.1777 0.8160 0.190 Uiso 1 1 calc GR . . . .
C02J C 0.4999(3) 0.3422(3) 0.6526(2) 0.1342(16) Uani 1 1 d . . . . .
H0BA H 0.4754 0.3582 0.6915 0.201 Uiso 1 1 calc GR . . . .
HQ H 0.4839 0.2720 0.6503 0.201 Uiso 1 1 calc GR . . . .
HR H 0.4655 0.3887 0.6257 0.201 Uiso 1 1 calc GR . . . .
C02K C 0.5124(3) 0.2864(3) 0.8882(3) 0.1445(19) Uani 1 1 d . . . . .
H02Y H 0.5206 0.3182 0.8484 0.217 Uiso 1 1 calc GR . . . .
HS H 0.5757 0.2471 0.8946 0.217 Uiso 1 1 calc GR . . . .
HT H 0.4990 0.3392 0.9136 0.217 Uiso 1 1 calc GR . . . .


_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
O001 H001 0.8200 . ?
O001 C00G 1.353(2) . ?
O002 H002 0.8200 . ?
O002 C00H 1.350(3) . ?
O003 H003 0.8200 . ?
O003 C00U 1.349(3) . ?
O004 H004 0.8200 . ?
O004 C00I 1.352(3) . ?
N005 C00R 1.463(3) . ?
N005 C00Z 1.457(3) . ?
N005 C010 1.453(3) . ?
O006 H006 0.8200 . ?
O006 C00T 1.349(3) . ?
O007 H007 0.8200 . ?
O007 C00X 1.347(3) . ?
N008 C01A 1.457(3) . ?
N008 C01D 1.449(3) . ?
N008 C01O 1.454(3) . ?
N009 C00F 1.270(3) . ?
N009 C00Q 1.456(3) . ?
N00A C00O 1.268(3) . ?
N00A C019 1.454(3) . ?
N00B C00S 1.270(3) . ?
N00B C01E 1.457(3) . ?
N00C C00K 1.262(3) . ?
N00C C014 1.450(3) . ?
N00D C00M 1.276(3) . ?
N00D C01U 1.439(3) . ?
N00E C012 1.265(3) . ?
N00E C01J 1.457(3) . ?
C00F H00F 0.9300 . ?
C00F C00N 1.457(3) . ?
C00G C00J 1.405(3) . ?
C00G C00L 1.402(3) . ?
C00H C00N 1.401(3) . ?
C00H C013 1.412(3) . ?
C00I C00P 1.400(3) . ?
C00I C011 1.406(3) . ?
C00J C018 1.535(3) . ?
C00J C01F 1.386(3) . ?
C00K H00K 0.9300 . ?
C00K C00W 1.458(3) . ?
C00L C00S 1.456(3) . ?
C00L C01H 1.390(3) . ?
C00M H00M 0.9300 . ?
C00M C00Y 1.454(3) . ?
C00N C00V 1.396(3) . ?
C00O H00O 0.9300 . ?
C00O C00P 1.461(3) . ?
C00P C01G 1.388(3) . ?
C00Q H00A 0.9700 . ?
C00Q H00B 0.9700 . ?
C00Q C00R 1.510(3) . ?
C00R H00C 0.9700 . ?
C00R H00D 0.9700 . ?
C00S H00S 0.9300 . ?
C00T C00Y 1.411(3) . ?
C00T C015 1.403(3) . ?
C00U C016 1.404(3) . ?
C00U C01I 1.408(3) . ?
C00V H00V 0.9300 . ?
C00V C01C 1.374(3) . ?
C00W C00X 1.400(3) . ?
C00W C01S 1.389(3) . ?
C00X C01M 1.413(3) . ?
C00Y C017 1.390(4) . ?
C00Z H00E 0.9700 . ?
C00Z H00G 0.9700 . ?
C00Z C019 1.512(4) . ?
C010 H01A 0.9700 . ?
C010 H01B 0.9700 . ?
C010 C01E 1.512(3) . ?
C011 C01L 1.387(4) . ?
C011 C01Y 1.531(4) . ?
C012 H012 0.9300 . ?
C012 C01I 1.465(4) . ?
C013 C01B 1.385(4) . ?
C013 C023 1.535(4) . ?
C014 H01M 0.9700 . ?
C014 H01N 0.9700 . ?
C014 C01D 1.504(3) . ?
C015 C01K 1.385(4) . ?
C015 C01P 1.531(3) . ?
C016 C01N 1.547(4) . ?
C016 C01X 1.390(4) . ?
C017 H017 0.9300 . ?
C017 C01R 1.368(4) . ?
C018 C021 1.531(4) . ?
C018 C022 1.536(4) . ?
C018 C029 1.522(4) . ?
C019 H01C 0.9700 . ?
C019 H01D 0.9700 . ?
C01A H01O 0.9700 . ?
C01A H01P 0.9700 . ?
C01A C01J 1.489(4) . ?
C01B H01E 0.9300 . ?
C01B C01C 1.379(4) . ?
C01C H01F 0.9300 . ?
C01D H01R 0.9700 . ?
C01D H01S 0.9700 . ?
C01E H01G 0.9700 . ?
C01E H01H 0.9700 . ?
C01F H01I 0.9300 . ?
C01F C01Q 1.383(4) . ?
C01G H01J 0.9300 . ?
C01G C01V 1.356(4) . ?
C01H H01K 0.9300 . ?
C01H C01Q 1.360(4) . ?
C01I C01W 1.390(4) . ?
C01J H01T 0.9700 . ?
C01J H01U 0.9700 . ?
C01K H01W 0.9300 . ?
C01K C01R 1.395(4) . ?
C01L H01L 0.9300 . ?
C01L C01V 1.385(4) . ?
C01M C01T 1.527(3) . ?
C01M C01Z 1.377(4) . ?
C01N C026 1.535(4) . ?
C01N C027 1.525(4) . ?
C01N C02E 1.522(4) . ?
C01O H01X 0.9700 . ?
C01O H01Y 0.9700 . ?
C01O C01U 1.502(4) . ?
C01P C020 1.545(4) . ?
C01P C02B 1.529(4) . ?
C01P C02C 1.527(4) . ?
C01Q H01Q 0.9300 . ?
C01R H01Z 0.9300 . ?
C01S H01 0.9300 . ?
C01S C025 1.370(4) . ?
C01T C024 1.532(4) . ?
C01T C02A 1.546(4) . ?
C01T C02J 1.513(5) . ?
C01U H0AA 0.9700 . ?
C01U H 0.9700 . ?
C01V H01V 0.9300 . ?
C01W H1AA 0.9300 . ?
C01W C028 1.373(5) . ?
C01X H2AA 0.9300 . ?
C01X C028 1.388(5) . ?
C01Y C02F 1.536(5) . ?
C01Y C02G 1.545(4) . ?
C01Y C02H 1.526(5) . ?
C01Z H3AA 0.9300 . ?
C01Z C025 1.382(4) . ?
C020 H02Z 0.9600 . ?
C020 HA 0.9600 . ?
C020 HB 0.9600 . ?
C021 H02A 0.9600 . ?
C021 H02B 0.9600 . ?
C021 H02C 0.9600 . ?
C022 H02D 0.9600 . ?
C022 H02E 0.9600 . ?
C022 H02F 0.9600 . ?
C023 C02D 1.542(6) . ?
C023 C02I 1.552(5) . ?
C023 C02K 1.537(4) . ?
C024 H02 0.9600 . ?
C024 HC 0.9600 . ?
C024 HD 0.9600 . ?
C025 H025 0.9300 . ?
C026 H4AA 0.9600 . ?
C026 HE 0.9600 . ?
C026 HF 0.9600 . ?
C027 H5AA 0.9600 . ?
C027 HG 0.9600 . ?
C027 HH 0.9600 . ?
C028 H028 0.9300 . ?
C029 H02G 0.9600 . ?
C029 H02H 0.9600 . ?
C029 H02I 0.9600 . ?
C02A H6AA 0.9600 . ?
C02A HI 0.9600 . ?
C02A HJ 0.9600 . ?
C02B H7AA 0.9600 . ?
C02B HK 0.9600 . ?
C02B HL 0.9600 . ?
C02C H8AA 0.9600 . ?
C02C HM 0.9600 . ?
C02C HN 0.9600 . ?
C02D H02J 0.9600 . ?
C02D H02K 0.9600 . ?
C02D H02L 0.9600 . ?
C02E H9AA 0.9600 . ?
C02E HO 0.9600 . ?
C02E HP 0.9600 . ?
C02F H02M 0.9600 . ?
C02F H02N 0.9600 . ?
C02F H02O 0.9600 . ?
C02G H02P 0.9600 . ?
C02G H02Q 0.9600 . ?
C02G H02R 0.9600 . ?
C02H H02S 0.9600 . ?
C02H H02T 0.9600 . ?
C02H H02U 0.9600 . ?
C02I H02V 0.9600 . ?
C02I H02W 0.9600 . ?
C02I H02X 0.9600 . ?
C02J H0BA 0.9600 . ?
C02J HQ 0.9600 . ?
C02J HR 0.9600 . ?
C02K H02Y 0.9600 . ?
C02K HS 0.9600 . ?
C02K HT 0.9600 . ?

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
C00G O001 H001 109.5 . . ?
C00H O002 H002 109.5 . . ?
C00U O003 H003 109.5 . . ?
C00I O004 H004 109.5 . . ?
C00Z N005 C00R 111.93(17) . . ?
C010 N005 C00R 111.44(17) . . ?
C010 N005 C00Z 110.83(18) . . ?
C00T O006 H006 109.5 . . ?
C00X O007 H007 109.5 . . ?
C01D N008 C01A 112.01(19) . . ?
C01D N008 C01O 110.2(2) . . ?
C01O N008 C01A 110.93(19) . . ?
C00F N009 C00Q 119.57(19) . . ?
C00O N00A C019 119.3(2) . . ?
C00S N00B C01E 120.2(2) . . ?
C00K N00C C014 119.7(2) . . ?
C00M N00D C01U 120.6(2) . . ?
C012 N00E C01J 120.9(2) . . ?
N009 C00F H00F 118.8 . . ?
N009 C00F C00N 122.4(2) . . ?
C00N C00F H00F 118.8 . . ?
O001 C00G C00J 119.2(2) . . ?
O001 C00G C00L 119.1(2) . . ?
C00L C00G C00J 121.70(19) . . ?
O002 C00H C00N 119.56(18) . . ?
O002 C00H C013 119.3(2) . . ?
C00N C00H C013 121.1(2) . . ?
O004 C00I C00P 119.27(19) . . ?
O004 C00I C011 119.6(2) . . ?
C00P C00I C011 121.1(2) . . ?
C00G C00J C018 121.84(19) . . ?
C01F C00J C00G 116.2(2) . . ?
C01F C00J C018 121.8(2) . . ?
N00C C00K H00K 118.4 . . ?
N00C C00K C00W 123.1(2) . . ?
C00W C00K H00K 118.4 . . ?
C00G C00L C00S 121.8(2) . . ?
C01H C00L C00G 119.2(2) . . ?
C01H C00L C00S 119.0(2) . . ?
N00D C00M H00M 118.9 . . ?
N00D C00M C00Y 122.3(2) . . ?
C00Y C00M H00M 118.9 . . ?
C00H C00N C00F 121.22(18) . . ?
C00V C00N C00F 118.7(2) . . ?
C00V C00N C00H 120.1(2) . . ?
N00A C00O H00O 118.6 . . ?
N00A C00O C00P 122.8(2) . . ?
C00P C00O H00O 118.6 . . ?
C00I C00P C00O 121.8(2) . . ?
C01G C00P C00I 119.8(2) . . ?
C01G C00P C00O 118.5(2) . . ?
N009 C00Q H00A 109.5 . . ?
N009 C00Q H00B 109.5 . . ?
N009 C00Q C00R 110.90(18) . . ?
H00A C00Q H00B 108.0 . . ?
C00R C00Q H00A 109.5 . . ?
C00R C00Q H00B 109.5 . . ?
N005 C00R C00Q 112.03(17) . . ?
N005 C00R H00C 109.2 . . ?
N005 C00R H00D 109.2 . . ?
C00Q C00R H00C 109.2 . . ?
C00Q C00R H00D 109.2 . . ?
H00C C00R H00D 107.9 . . ?
N00B C00S C00L 122.9(2) . . ?
N00B C00S H00S 118.6 . . ?
C00L C00S H00S 118.6 . . ?
O006 C00T C00Y 119.4(2) . . ?
O006 C00T C015 119.5(2) . . ?
C015 C00T C00Y 121.1(2) . . ?
O003 C00U C016 119.6(2) . . ?
O003 C00U C01I 119.2(2) . . ?
C016 C00U C01I 121.3(2) . . ?
C00N C00V H00V 120.3 . . ?
C01C C00V C00N 119.4(2) . . ?
C01C C00V H00V 120.3 . . ?
C00X C00W C00K 121.9(2) . . ?
C01S C00W C00K 118.7(2) . . ?
C01S C00W C00X 119.4(2) . . ?
O007 C00X C00W 119.7(2) . . ?
O007 C00X C01M 119.2(2) . . ?
C00W C00X C01M 121.0(2) . . ?
C00T C00Y C00M 121.0(2) . . ?
C017 C00Y C00M 119.0(2) . . ?
C017 C00Y C00T 120.0(2) . . ?
N005 C00Z H00E 109.0 . . ?
N005 C00Z H00G 109.0 . . ?
N005 C00Z C019 112.84(19) . . ?
H00E C00Z H00G 107.8 . . ?
C019 C00Z H00E 109.0 . . ?
C019 C00Z H00G 109.0 . . ?
N005 C010 H01A 109.0 . . ?
N005 C010 H01B 109.0 . . ?
N005 C010 C01E 112.84(19) . . ?
H01A C010 H01B 107.8 . . ?
C01E C010 H01A 109.0 . . ?
C01E C010 H01B 109.0 . . ?
C00I C011 C01Y 121.4(2) . . ?
C01L C011 C00I 116.0(2) . . ?
C01L C011 C01Y 122.6(2) . . ?
N00E C012 H012 118.9 . . ?
N00E C012 C01I 122.3(2) . . ?
C01I C012 H012 118.9 . . ?
C00H C013 C023 121.4(2) . . ?
C01B C013 C00H 115.9(2) . . ?
C01B C013 C023 122.7(2) . . ?
N00C C014 H01M 109.2 . . ?
N00C C014 H01N 109.2 . . ?
N00C C014 C01D 112.23(19) . . ?
H01M C014 H01N 107.9 . . ?
C01D C014 H01M 109.2 . . ?
C01D C014 H01N 109.2 . . ?
C00T C015 C01P 121.8(2) . . ?
C01K C015 C00T 116.5(2) . . ?
C01K C015 C01P 121.7(2) . . ?
C00U C016 C01N 121.9(2) . . ?
C01X C016 C00U 116.0(2) . . ?
C01X C016 C01N 122.1(2) . . ?
C00Y C017 H017 120.2 . . ?
C01R C017 C00Y 119.6(2) . . ?
C01R C017 H017 120.2 . . ?
C00J C018 C022 110.5(2) . . ?
C021 C018 C00J 108.7(2) . . ?
C021 C018 C022 110.1(3) . . ?
C029 C018 C00J 112.8(2) . . ?
C029 C018 C021 108.2(3) . . ?
C029 C018 C022 106.6(3) . . ?
N00A C019 C00Z 110.5(2) . . ?
N00A C019 H01C 109.5 . . ?
N00A C019 H01D 109.5 . . ?
C00Z C019 H01C 109.5 . . ?
C00Z C019 H01D 109.5 . . ?
H01C C019 H01D 108.1 . . ?
N008 C01A H01O 108.8 . . ?
N008 C01A H01P 108.8 . . ?
N008 C01A C01J 113.9(2) . . ?
H01O C01A H01P 107.7 . . ?
C01J C01A H01O 108.8 . . ?
C01J C01A H01P 108.8 . . ?
C013 C01B H01E 118.0 . . ?
C01C C01B C013 123.9(2) . . ?
C01C C01B H01E 118.0 . . ?
C00V C01C C01B 119.6(2) . . ?
C00V C01C H01F 120.2 . . ?
C01B C01C H01F 120.2 . . ?
N008 C01D C014 113.3(2) . . ?
N008 C01D H01R 108.9 . . ?
N008 C01D H01S 108.9 . . ?
C014 C01D H01R 108.9 . . ?
C014 C01D H01S 108.9 . . ?
H01R C01D H01S 107.7 . . ?
N00B C01E C010 110.8(2) . . ?
N00B C01E H01G 109.5 . . ?
N00B C01E H01H 109.5 . . ?
C010 C01E H01G 109.5 . . ?
C010 C01E H01H 109.5 . . ?
H01G C01E H01H 108.1 . . ?
C00J C01F H01I 118.8 . . ?
C01Q C01F C00J 122.5(3) . . ?
C01Q C01F H01I 118.8 . . ?
C00P C01G H01J 119.9 . . ?
C01V C01G C00P 120.3(3) . . ?
C01V C01G H01J 119.9 . . ?
C00L C01H H01K 120.0 . . ?
C01Q C01H C00L 119.9(2) . . ?
C01Q C01H H01K 120.0 . . ?
C00U C01I C012 121.0(2) . . ?
C01W C01I C00U 120.1(3) . . ?
C01W C01I C012 118.9(2) . . ?
N00E C01J C01A 111.3(2) . . ?
N00E C01J H01T 109.4 . . ?
N00E C01J H01U 109.4 . . ?
C01A C01J H01T 109.4 . . ?
C01A C01J H01U 109.4 . . ?
H01T C01J H01U 108.0 . . ?
C015 C01K H01W 118.5 . . ?
C015 C01K C01R 123.0(3) . . ?
C01R C01K H01W 118.5 . . ?
C011 C01L H01L 118.3 . . ?
C01V C01L C011 123.4(2) . . ?
C01V C01L H01L 118.3 . . ?
C00X C01M C01T 121.9(2) . . ?
C01Z C01M C00X 116.6(2) . . ?
C01Z C01M C01T 121.5(2) . . ?
C026 C01N C016 109.3(2) . . ?
C027 C01N C016 110.1(2) . . ?
C027 C01N C026 109.8(3) . . ?
C02E C01N C016 112.3(3) . . ?
C02E C01N C026 108.6(3) . . ?
C02E C01N C027 106.6(3) . . ?
N008 C01O H01X 109.0 . . ?
N008 C01O H01Y 109.0 . . ?
N008 C01O C01U 113.0(2) . . ?
H01X C01O H01Y 107.8 . . ?
C01U C01O H01X 109.0 . . ?
C01U C01O H01Y 109.0 . . ?
C015 C01P C020 110.1(2) . . ?
C02B C01P C015 109.7(2) . . ?
C02B C01P C020 108.9(3) . . ?
C02C C01P C015 112.0(2) . . ?
C02C C01P C020 107.4(2) . . ?
C02C C01P C02B 108.6(3) . . ?
C01F C01Q H01Q 119.7 . . ?
C01H C01Q C01F 120.5(2) . . ?
C01H C01Q H01Q 119.7 . . ?
C017 C01R C01K 119.8(3) . . ?
C017 C01R H01Z 120.1 . . ?
C01K C01R H01Z 120.1 . . ?
C00W C01S H01 119.8 . . ?
C025 C01S C00W 120.4(2) . . ?
C025 C01S H01 119.8 . . ?
C01M C01T C024 111.7(2) . . ?
C01M C01T C02A 108.1(2) . . ?
C024 C01T C02A 106.3(2) . . ?
C02J C01T C01M 110.9(2) . . ?
C02J C01T C024 107.4(3) . . ?
C02J C01T C02A 112.4(3) . . ?
N00D C01U C01O 110.9(2) . . ?
N00D C01U H0AA 109.5 . . ?
N00D C01U H 109.5 . . ?
C01O C01U H0AA 109.5 . . ?
C01O C01U H 109.5 . . ?
H0AA C01U H 108.0 . . ?
C01G C01V C01L 119.5(2) . . ?
C01G C01V H01V 120.3 . . ?
C01L C01V H01V 120.3 . . ?
C01I C01W H1AA 120.2 . . ?
C028 C01W C01I 119.5(3) . . ?
C028 C01W H1AA 120.2 . . ?
C016 C01X H2AA 118.3 . . ?
C028 C01X C016 123.5(3) . . ?
C028 C01X H2AA 118.3 . . ?
C011 C01Y C02F 109.3(3) . . ?
C011 C01Y C02G 111.1(3) . . ?
C02F C01Y C02G 106.5(3) . . ?
C02H C01Y C011 109.9(3) . . ?
C02H C01Y C02F 111.8(3) . . ?
C02H C01Y C02G 108.3(3) . . ?
C01M C01Z H3AA 118.4 . . ?
C01M C01Z C025 123.2(2) . . ?
C025 C01Z H3AA 118.4 . . ?
C01P C020 H02Z 109.5 . . ?
C01P C020 HA 109.5 . . ?
C01P C020 HB 109.5 . . ?
H02Z C020 HA 109.5 . . ?
H02Z C020 HB 109.5 . . ?
HA C020 HB 109.5 . . ?
C018 C021 H02A 109.5 . . ?
C018 C021 H02B 109.5 . . ?
C018 C021 H02C 109.5 . . ?
H02A C021 H02B 109.5 . . ?
H02A C021 H02C 109.5 . . ?
H02B C021 H02C 109.5 . . ?
C018 C022 H02D 109.5 . . ?
C018 C022 H02E 109.5 . . ?
C018 C022 H02F 109.5 . . ?
H02D C022 H02E 109.5 . . ?
H02D C022 H02F 109.5 . . ?
H02E C022 H02F 109.5 . . ?
C013 C023 C02D 110.9(3) . . ?
C013 C023 C02I 108.0(3) . . ?
C013 C023 C02K 111.3(3) . . ?
C02D C023 C02I 111.3(3) . . ?
C02K C023 C02D 107.5(3) . . ?
C02K C023 C02I 107.7(3) . . ?
C01T C024 H02 109.5 . . ?
C01T C024 HC 109.5 . . ?
C01T C024 HD 109.5 . . ?
H02 C024 HC 109.5 . . ?
H02 C024 HD 109.5 . . ?
HC C024 HD 109.5 . . ?
C01S C025 C01Z 119.4(3) . . ?
C01S C025 H025 120.3 . . ?
C01Z C025 H025 120.3 . . ?
C01N C026 H4AA 109.5 . . ?
C01N C026 HE 109.5 . . ?
C01N C026 HF 109.5 . . ?
H4AA C026 HE 109.5 . . ?
H4AA C026 HF 109.5 . . ?
HE C026 HF 109.5 . . ?
C01N C027 H5AA 109.5 . . ?
C01N C027 HG 109.5 . . ?
C01N C027 HH 109.5 . . ?
H5AA C027 HG 109.5 . . ?
H5AA C027 HH 109.5 . . ?
HG C027 HH 109.5 . . ?
C01W C028 C01X 119.6(3) . . ?
C01W C028 H028 120.2 . . ?
C01X C028 H028 120.2 . . ?
C018 C029 H02G 109.5 . . ?
C018 C029 H02H 109.5 . . ?
C018 C029 H02I 109.5 . . ?
H02G C029 H02H 109.5 . . ?
H02G C029 H02I 109.5 . . ?
H02H C029 H02I 109.5 . . ?
C01T C02A H6AA 109.5 . . ?
C01T C02A HI 109.5 . . ?
C01T C02A HJ 109.5 . . ?
H6AA C02A HI 109.5 . . ?
H6AA C02A HJ 109.5 . . ?
HI C02A HJ 109.5 . . ?
C01P C02B H7AA 109.5 . . ?
C01P C02B HK 109.5 . . ?
C01P C02B HL 109.5 . . ?
H7AA C02B HK 109.5 . . ?
H7AA C02B HL 109.5 . . ?
HK C02B HL 109.5 . . ?
C01P C02C H8AA 109.5 . . ?
C01P C02C HM 109.5 . . ?
C01P C02C HN 109.5 . . ?
H8AA C02C HM 109.5 . . ?
H8AA C02C HN 109.5 . . ?
HM C02C HN 109.5 . . ?
C023 C02D H02J 109.5 . . ?
C023 C02D H02K 109.5 . . ?
C023 C02D H02L 109.5 . . ?
H02J C02D H02K 109.5 . . ?
H02J C02D H02L 109.5 . . ?
H02K C02D H02L 109.5 . . ?
C01N C02E H9AA 109.5 . . ?
C01N C02E HO 109.5 . . ?
C01N C02E HP 109.5 . . ?
H9AA C02E HO 109.5 . . ?
H9AA C02E HP 109.5 . . ?
HO C02E HP 109.5 . . ?
C01Y C02F H02M 109.5 . . ?
C01Y C02F H02N 109.5 . . ?
C01Y C02F H02O 109.5 . . ?
H02M C02F H02N 109.5 . . ?
H02M C02F H02O 109.5 . . ?
H02N C02F H02O 109.5 . . ?
C01Y C02G H02P 109.5 . . ?
C01Y C02G H02Q 109.5 . . ?
C01Y C02G H02R 109.5 . . ?
H02P C02G H02Q 109.5 . . ?
H02P C02G H02R 109.5 . . ?
H02Q C02G H02R 109.5 . . ?
C01Y C02H H02S 109.5 . . ?
C01Y C02H H02T 109.5 . . ?
C01Y C02H H02U 109.5 . . ?
H02S C02H H02T 109.5 . . ?
H02S C02H H02U 109.5 . . ?
H02T C02H H02U 109.5 . . ?
C023 C02I H02V 109.5 . . ?
C023 C02I H02W 109.5 . . ?
C023 C02I H02X 109.5 . . ?
H02V C02I H02W 109.5 . . ?
H02V C02I H02X 109.5 . . ?
H02W C02I H02X 109.5 . . ?
C01T C02J H0BA 109.5 . . ?
C01T C02J HQ 109.5 . . ?
C01T C02J HR 109.5 . . ?
H0BA C02J HQ 109.5 . . ?
H0BA C02J HR 109.5 . . ?
HQ C02J HR 109.5 . . ?
C023 C02K H02Y 109.5 . . ?
C023 C02K HS 109.5 . . ?
C023 C02K HT 109.5 . . ?
H02Y C02K HS 109.5 . . ?
H02Y C02K HT 109.5 . . ?
HS C02K HT 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-23
_olex2_submission_special_instructions 'No special instructions were received'
