# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

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

data_md15-n2-a
_database_code_depnum_ccdc_archive 'CCDC 1812145'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48.50 H59 Cl N11'
_chemical_formula_weight         831.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.8594(6)
_cell_length_b                   13.3077(7)
_cell_length_c                   15.7675(8)
_cell_angle_alpha                105.058(4)
_cell_angle_beta                 101.304(4)
_cell_angle_gamma                96.287(4)
_cell_volume                     2322.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    3681
_cell_measurement_theta_min      3.850
_cell_measurement_theta_max      24.282

_exptl_crystal_description       'distrorted cube'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 0 1 0.0350 0.0016 0.0014 0.9940 -0.0112 -0.0441 -0.0142
0 0 -1 0.0550 -0.0016 -0.0014 -0.9940 0.0112 0.0441 0.0142
1 0 0 0.0500 0.9887 0.0046 0.0020 0.0316 -0.0361 0.0381
-1 0 0 0.0500 -0.9887 -0.0046 -0.0020 -0.0316 0.0361 -0.0381
0 1 0 0.0700 0.0012 0.9948 -0.0030 -0.0412 -0.0175 0.0332
0 -1 0 0.0600 -0.0012 -0.9948 0.0030 0.0412 0.0175 -0.0332
1 0 -1 0.0600 0.9871 0.0032 -0.9920 0.0428 0.0080 0.0523
-1 0 1 0.0550 -0.9871 -0.0032 0.9920 -0.0428 -0.0080 -0.0523
0 1 -1 0.0950 -0.0004 0.9935 -0.9970 -0.0299 0.0266 0.0473
-1 1 0 0.0800 -0.9875 0.9902 -0.0050 -0.0728 0.0185 -0.0050
1 -1 0 0.0750 0.9875 -0.9902 0.0050 0.0728 -0.0185 0.0050
_exptl_absorpt_coefficient_mu    0.128
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.33450
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_reflns_number            16755
_diffrn_reflns_av_unetI/netI     0.1479
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.217
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_orient_matrix_UB_11      0.0321716000
_diffrn_orient_matrix_UB_12      -0.0414455000
_diffrn_orient_matrix_UB_13      -0.0112751000
_diffrn_orient_matrix_UB_21      -0.0363162000
_diffrn_orient_matrix_UB_22      -0.0177207000
_diffrn_orient_matrix_UB_23      -0.0442925000
_diffrn_orient_matrix_UB_31      0.0384204000
_diffrn_orient_matrix_UB_32      0.0332383000
_diffrn_orient_matrix_UB_33      -0.0143775000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -36.00   61.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7155   77.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega  -13.00  103.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6530   77.0000  120.0000 116

#__ type_ start__ end____ width___ exp.time_
  3 omega    4.00   55.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6530   77.0000 -150.0000 51

#__ type_ start__ end____ width___ exp.time_
  4 omega  -14.00   99.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6530   77.0000    0.0000 113

;
_reflns_number_total             9473
_reflns_number_gt                4756
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;

_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;

_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;

_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
WinGX Version 2014.12, J.L. Farrugia, 212, J Appl. Cryst. 45, 849-854
;
_computing_publication_material  ?
_refine_special_details          
;
Refined as a 2-component perfect inversion twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1604P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0000(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9473
_refine_ls_number_parameters     573
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.0924
_refine_ls_wR_factor_ref         0.3208
_refine_ls_wR_factor_gt          0.2518
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.242
_refine_ls_shift/su_mean         0.001

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
C1 C 0.5364(3) 0.3321(3) 0.6785(2) 0.0362(9) Uani 1 1 d . . . . .
H1 H 0.5205 0.2709 0.7027 0.043 Uiso 1 1 calc R U . . .
C2 C 0.4363(3) 0.3954(3) 0.6880(2) 0.0370(9) Uani 1 1 d . . . . .
C3 C 0.3457(4) 0.3641(3) 0.7255(3) 0.0439(10) Uani 1 1 d . . . . .
H3 H 0.3465 0.3032 0.7462 0.053 Uiso 1 1 calc R U . . .
C4 C 0.2559(4) 0.4199(3) 0.7328(3) 0.0481(11) Uani 1 1 d . . . . .
H4 H 0.1943 0.3969 0.7574 0.058 Uiso 1 1 calc R U . . .
C5 C 0.2549(4) 0.5104(3) 0.7038(3) 0.0446(10) Uani 1 1 d . . . . .
C6 C 0.3447(4) 0.5439(3) 0.6678(3) 0.0438(10) Uani 1 1 d . . . . .
H6 H 0.3445 0.6055 0.6481 0.053 Uiso 1 1 calc R U . . .
C7 C 0.4346(4) 0.4861(3) 0.6609(3) 0.0413(10) Uani 1 1 d . . . . .
H7 H 0.4967 0.5095 0.6370 0.050 Uiso 1 1 calc R U . . .
C8 C 0.1652(5) 0.6611(4) 0.6944(4) 0.0674(14) Uani 1 1 d . . . . .
H8A H 0.2340 0.7112 0.7335 0.101 Uiso 1 1 calc R U . . .
H8B H 0.0944 0.6894 0.7045 0.101 Uiso 1 1 calc R U . . .
H8C H 0.1682 0.6502 0.6311 0.101 Uiso 1 1 calc R U . . .
C9 C 0.5338(3) 0.2868(3) 0.5791(3) 0.0386(9) Uani 1 1 d . . . . .
C10 C 0.4731(3) 0.1925(3) 0.5235(3) 0.0377(9) Uani 1 1 d . . . . .
C11 C 0.5786(4) 0.3363(3) 0.5194(3) 0.0407(9) Uani 1 1 d . . . . .
H11 H 0.6246 0.4048 0.5389 0.049 Uiso 1 1 calc R U . . .
C12 C 0.3672(3) 0.0438(3) 0.4424(3) 0.0387(9) Uani 1 1 d . . . . .
C13 C 0.4140(3) 0.0934(3) 0.3767(3) 0.0374(9) Uani 1 1 d . . . . .
C14 C 0.4269(4) 0.1010(3) 0.2242(3) 0.0421(10) Uani 1 1 d . . . . .
C15 C 0.5610(3) 0.1111(3) 0.2358(3) 0.0418(9) Uani 1 1 d . . . . .
H15A H 0.5835 0.1603 0.2021 0.050 Uiso 1 1 calc R U . . .
H15B H 0.5967 0.1467 0.3005 0.050 Uiso 1 1 calc R U . . .
C16 C 0.6215(4) 0.0146(3) 0.2082(3) 0.0450(10) Uani 1 1 d . . . . .
C17 C 0.3943(4) 0.2106(3) 0.2355(3) 0.0484(11) Uani 1 1 d . . . . .
H17A H 0.3103 0.2060 0.2316 0.073 Uiso 1 1 calc R U . . .
H17B H 0.4142 0.2385 0.1876 0.073 Uiso 1 1 calc R U . . .
H17C H 0.4375 0.2577 0.2945 0.073 Uiso 1 1 calc R U . . .
C18 C 0.3560(4) 0.0304(3) 0.1325(3) 0.0486(11) Uani 1 1 d . . . . .
H18A H 0.3662 -0.0430 0.1268 0.073 Uiso 1 1 calc R U . . .
H18B H 0.3829 0.0531 0.0844 0.073 Uiso 1 1 calc R U . . .
H18C H 0.2733 0.0356 0.1272 0.073 Uiso 1 1 calc R U . . .
C19 C 0.7526(4) 0.0492(4) 0.2525(3) 0.0548(12) Uani 1 1 d . . . . .
H19A H 0.7928 -0.0115 0.2385 0.082 Uiso 1 1 calc R U . . .
H19B H 0.7637 0.0767 0.3180 0.082 Uiso 1 1 calc R U . . .
H19C H 0.7848 0.1045 0.2289 0.082 Uiso 1 1 calc R U . . .
C20 C 0.5764(4) -0.0793(3) 0.2396(3) 0.0551(12) Uani 1 1 d . . . . .
H20A H 0.4949 -0.1073 0.2076 0.083 Uiso 1 1 calc R U . . .
H20B H 0.5818 -0.0557 0.3048 0.083 Uiso 1 1 calc R U . . .
H20C H 0.6239 -0.1347 0.2265 0.083 Uiso 1 1 calc R U . . .
C21 C 0.6101(5) -0.0219(4) 0.1051(3) 0.0632(13) Uani 1 1 d . . . . .
H21A H 0.5290 -0.0539 0.0744 0.095 Uiso 1 1 calc R U . . .
H21B H 0.6611 -0.0740 0.0910 0.095 Uiso 1 1 calc R U . . .
H21C H 0.6330 0.0390 0.0844 0.095 Uiso 1 1 calc R U . . .
C22 C 0.2902(3) -0.0584(3) 0.4191(3) 0.0372(9) Uani 1 1 d . . . . .
C23 C 0.2695(4) -0.1004(3) 0.4883(3) 0.0467(10) Uani 1 1 d . . . . .
H23 H 0.3056 -0.0616 0.5490 0.056 Uiso 1 1 calc R U . . .
C24 C 0.1992(4) -0.1955(3) 0.4717(3) 0.0451(10) Uani 1 1 d . . . . .
H24 H 0.1869 -0.2220 0.5202 0.054 Uiso 1 1 calc R U . . .
C25 C 0.1459(4) -0.2528(3) 0.3828(3) 0.0486(11) Uani 1 1 d . . . . .
C26 C 0.1647(4) -0.2130(3) 0.3141(3) 0.0519(11) Uani 1 1 d . . . . .
H26 H 0.1280 -0.2525 0.2536 0.062 Uiso 1 1 calc R U . . .
C27 C 0.2349(4) -0.1179(3) 0.3296(3) 0.0467(10) Uani 1 1 d . . . . .
H27 H 0.2461 -0.0923 0.2804 0.056 Uiso 1 1 calc R U . . .
C28 C 0.0640(5) -0.3963(4) 0.4279(4) 0.0690(15) Uani 1 1 d . . . . .
H28A H 0.1414 -0.3998 0.4618 0.103 Uiso 1 1 calc R U . . .
H28B H 0.0191 -0.4679 0.4008 0.103 Uiso 1 1 calc R U . . .
H28C H 0.0231 -0.3542 0.4688 0.103 Uiso 1 1 calc R U . . .
C29 C 0.6510(3) 0.3969(3) 0.7355(3) 0.0389(9) Uani 1 1 d . . . . .
C30 C 0.7178(3) 0.4818(3) 0.7266(3) 0.0390(9) Uani 1 1 d . . . . .
C31 C 0.7111(4) 0.3901(3) 0.8221(3) 0.0458(10) Uani 1 1 d . . . . .
H31 H 0.6851 0.3377 0.8482 0.055 Uiso 1 1 calc R U . . .
C32 C 0.8106(3) 0.6186(3) 0.7039(3) 0.0377(9) Uani 1 1 d . . . . .
C33 C 0.8760(3) 0.6122(3) 0.7951(3) 0.0374(9) Uani 1 1 d . . . . .
C34 C 1.0401(4) 0.6719(3) 0.9289(3) 0.0474(10) Uani 1 1 d . . . . .
C35 C 0.9751(4) 0.6829(3) 1.0057(3) 0.0468(10) Uani 1 1 d . . . . .
H35A H 0.9097 0.6227 0.9850 0.056 Uiso 1 1 calc R U . . .
H35B H 1.0294 0.6714 1.0572 0.056 Uiso 1 1 calc R U . . .
C36 C 0.9241(5) 0.7814(4) 1.0444(3) 0.0608(13) Uani 1 1 d . . . . .
C37 C 1.0833(4) 0.5658(4) 0.9135(3) 0.0596(13) Uani 1 1 d . . . . .
H37A H 1.0179 0.5092 0.9040 0.089 Uiso 1 1 calc R U . . .
H37B H 1.1434 0.5673 0.9665 0.089 Uiso 1 1 calc R U . . .
H37C H 1.1164 0.5530 0.8601 0.089 Uiso 1 1 calc R U . . .
C38 C 1.1448(4) 0.7596(4) 0.9485(3) 0.0682(15) Uani 1 1 d . . . . .
H38A H 1.1920 0.7394 0.9043 0.102 Uiso 1 1 calc R U . . .
H38B H 1.1923 0.7703 1.0094 0.102 Uiso 1 1 calc R U . . .
H38C H 1.1171 0.8253 0.9443 0.102 Uiso 1 1 calc R U . . .
C39 C 0.8411(6) 0.8103(5) 0.9711(4) 0.088(2) Uani 1 1 d . . . . .
H39A H 0.7761 0.7516 0.9412 0.131 Uiso 1 1 calc R U . . .
H39B H 0.8831 0.8244 0.9266 0.131 Uiso 1 1 calc R U . . .
H39C H 0.8108 0.8735 0.9983 0.131 Uiso 1 1 calc R U . . .
C40 C 1.0180(6) 0.8773(4) 1.0991(4) 0.093(2) Uani 1 1 d . . . . .
H40A H 0.9843 0.9274 1.1402 0.140 Uiso 1 1 calc R U . . .
H40B H 1.0470 0.9117 1.0578 0.140 Uiso 1 1 calc R U . . .
H40C H 1.0826 0.8542 1.1341 0.140 Uiso 1 1 calc R U . . .
C41 C 0.8562(5) 0.7526(5) 1.1119(3) 0.0754(16) Uani 1 1 d . . . . .
H41A H 0.7928 0.6932 1.0795 0.113 Uiso 1 1 calc R U . . .
H41B H 0.8236 0.8137 1.1405 0.113 Uiso 1 1 calc R U . . .
H41C H 0.9093 0.7327 1.1584 0.113 Uiso 1 1 calc R U . . .
C42 C 0.8404(3) 0.6957(3) 0.6580(3) 0.0376(9) Uani 1 1 d . . . . .
C43 C 0.7953(4) 0.6714(3) 0.5658(3) 0.0445(10) Uani 1 1 d . . . . .
H43 H 0.7478 0.6045 0.5351 0.053 Uiso 1 1 calc R U . . .
C44 C 0.8166(4) 0.7401(3) 0.5168(3) 0.0473(10) Uani 1 1 d . . . . .
H44 H 0.7836 0.7210 0.4536 0.057 Uiso 1 1 calc R U . . .
C45 C 0.8862(4) 0.8372(3) 0.5602(3) 0.0443(10) Uani 1 1 d . . . . .
C46 C 0.9298(4) 0.8656(3) 0.6537(3) 0.0464(10) Uani 1 1 d . . . . .
H46 H 0.9746 0.9336 0.6846 0.056 Uiso 1 1 calc R U . . .
C47 C 0.9079(4) 0.7950(3) 0.7008(3) 0.0449(10) Uani 1 1 d . . . . .
H47 H 0.9395 0.8145 0.7642 0.054 Uiso 1 1 calc R U . . .
C48 C 0.8754(4) 0.8823(4) 0.4214(3) 0.0583(12) Uani 1 1 d . . . . .
H48A H 0.9032 0.8177 0.3940 0.087 Uiso 1 1 calc R U . . .
H48B H 0.9056 0.9397 0.3992 0.087 Uiso 1 1 calc R U . . .
H48C H 0.7899 0.8702 0.4051 0.087 Uiso 1 1 calc R U . . .
N1 N 0.1635(3) 0.5632(2) 0.7151(2) 0.0379(8) Uani 1 1 d . . . . .
N2 N 0.4842(3) 0.1873(2) 0.4375(2) 0.0391(8) Uani 1 1 d . . . . .
N3 N 0.5495(3) 0.2773(2) 0.4340(2) 0.0429(8) Uani 1 1 d . . . . .
N4 N 0.4039(3) 0.1029(2) 0.5259(2) 0.0370(7) Uani 1 1 d . . . . .
N5 N 0.3889(3) 0.0542(2) 0.2917(2) 0.0409(8) Uani 1 1 d . . . . .
N6 N 0.0761(3) -0.3487(2) 0.3585(2) 0.0447(9) Uani 1 1 d . . . . .
N7 N 0.8080(3) 0.5198(2) 0.8015(2) 0.0418(8) Uani 1 1 d . . . . .
N8 N 0.8053(3) 0.4626(3) 0.8623(2) 0.0467(9) Uani 1 1 d . . . . .
N9 N 0.7204(3) 0.5430(2) 0.6669(2) 0.0393(8) Uani 1 1 d . . . . .
N10 N 0.9664(3) 0.6763(3) 0.8432(2) 0.0430(8) Uani 1 1 d . . . . .
N11 N 0.9161(3) 0.9111(2) 0.5192(2) 0.0373(8) Uani 1 1 d . . . . .
Cl1 Cl 0.5743(3) 0.5652(2) 0.9222(2) 0.0939(10) Uani 0.5 1 d D . P . .
Cl2 Cl 0.4615(3) 0.7233(2) 1.0047(4) 0.1344(19) Uani 0.5 1 d D . P . .
C49 C 0.4482(9) 0.6131(10) 0.9258(7) 0.122(6) Uani 0.5 1 d D . P . .
H49A H 0.4165 0.6243 0.8667 0.147 Uiso 0.5 1 calc R U P . .
H49B H 0.3909 0.5594 0.9350 0.147 Uiso 0.5 1 calc R U P . .


_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
C1 C29 1.503(5) . ?
C1 C9 1.519(5) . ?
C1 C2 1.537(5) . ?
C1 H1 1.0000 . ?
C2 C7 1.382(5) . ?
C2 C3 1.398(5) . ?
C3 C4 1.370(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(6) . ?
C4 H4 0.9500 . ?
C5 N1 1.371(5) . ?
C5 C6 1.385(6) . ?
C6 C7 1.386(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 N1 1.423(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.358(5) . ?
C9 C11 1.429(5) . ?
C10 N2 1.374(5) . ?
C10 N4 1.385(5) . ?
C11 N3 1.326(5) . ?
C11 H11 0.9500 . ?
C12 N4 1.305(5) . ?
C12 C22 1.468(5) . ?
C12 C13 1.523(5) . ?
C13 N5 1.265(5) . ?
C13 N2 1.417(5) . ?
C14 N5 1.482(5) . ?
C14 C17 1.525(5) . ?
C14 C18 1.526(5) . ?
C14 C15 1.551(6) . ?
C15 C16 1.545(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C19 1.539(6) . ?
C16 C20 1.540(6) . ?
C16 C21 1.545(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.398(6) . ?
C22 C27 1.412(5) . ?
C23 C24 1.370(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.392(6) . ?
C24 H24 0.9500 . ?
C25 N6 1.361(5) . ?
C25 C26 1.367(6) . ?
C26 C27 1.372(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 N6 1.421(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.361(5) . ?
C29 C31 1.442(5) . ?
C30 N7 1.368(5) . ?
C30 N9 1.398(5) . ?
C31 N8 1.323(5) . ?
C31 H31 0.9500 . ?
C32 N9 1.308(5) . ?
C32 C42 1.453(5) . ?
C32 C33 1.523(5) . ?
C33 N10 1.264(5) . ?
C33 N7 1.432(5) . ?
C34 N10 1.477(5) . ?
C34 C37 1.531(6) . ?
C34 C38 1.532(6) . ?
C34 C35 1.542(6) . ?
C35 C36 1.536(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C39 1.524(7) . ?
C36 C40 1.534(8) . ?
C36 C41 1.552(7) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.385(6) . ?
C42 C47 1.392(5) . ?
C43 C44 1.375(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.380(6) . ?
C44 H44 0.9500 . ?
C45 N11 1.362(5) . ?
C45 C46 1.398(6) . ?
C46 C47 1.374(6) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 N11 1.457(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N2 N3 1.373(4) . ?
N7 N8 1.373(4) . ?
Cl1 C49 1.693(10) . ?
Cl2 C49 1.627(10) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C29 C1 C9 114.9(3) . . ?
C29 C1 C2 110.9(3) . . ?
C9 C1 C2 109.5(3) . . ?
C29 C1 H1 107.1 . . ?
C9 C1 H1 107.1 . . ?
C2 C1 H1 107.1 . . ?
C7 C2 C3 118.1(4) . . ?
C7 C2 C1 120.7(3) . . ?
C3 C2 C1 121.2(3) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C6 123.4(4) . . ?
N1 C5 C4 116.5(4) . . ?
C6 C5 C4 120.1(4) . . ?
C5 C6 C7 119.0(4) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C2 C7 C6 121.8(4) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C11 103.7(3) . . ?
C10 C9 C1 126.4(4) . . ?
C11 C9 C1 129.4(3) . . ?
C9 C10 N2 107.7(3) . . ?
C9 C10 N4 140.6(4) . . ?
N2 C10 N4 111.7(3) . . ?
N3 C11 C9 113.4(3) . . ?
N3 C11 H11 123.3 . . ?
C9 C11 H11 123.3 . . ?
N4 C12 C22 121.5(3) . . ?
N4 C12 C13 112.2(3) . . ?
C22 C12 C13 126.3(3) . . ?
N5 C13 N2 134.5(4) . . ?
N5 C13 C12 125.0(3) . . ?
N2 C13 C12 100.5(3) . . ?
N5 C14 C17 110.1(3) . . ?
N5 C14 C18 105.5(3) . . ?
C17 C14 C18 107.4(3) . . ?
N5 C14 C15 110.8(3) . . ?
C17 C14 C15 108.5(3) . . ?
C18 C14 C15 114.3(3) . . ?
C16 C15 C14 122.5(3) . . ?
C16 C15 H15A 106.7 . . ?
C14 C15 H15A 106.7 . . ?
C16 C15 H15B 106.7 . . ?
C14 C15 H15B 106.7 . . ?
H15A C15 H15B 106.6 . . ?
C19 C16 C20 108.0(4) . . ?
C19 C16 C15 107.7(3) . . ?
C20 C16 C15 113.2(3) . . ?
C19 C16 C21 106.6(4) . . ?
C20 C16 C21 109.5(4) . . ?
C15 C16 C21 111.4(3) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C27 117.3(3) . . ?
C23 C22 C12 119.2(4) . . ?
C27 C22 C12 123.5(4) . . ?
C24 C23 C22 122.5(4) . . ?
C24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C23 C24 C25 119.0(4) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
N6 C25 C26 116.6(4) . . ?
N6 C25 C24 124.0(4) . . ?
C26 C25 C24 119.4(4) . . ?
C25 C26 C27 122.3(4) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C26 C27 C22 119.5(4) . . ?
C26 C27 H27 120.3 . . ?
C22 C27 H27 120.3 . . ?
N6 C28 H28A 109.5 . . ?
N6 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N6 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C31 102.0(3) . . ?
C30 C29 C1 131.2(3) . . ?
C31 C29 C1 126.5(4) . . ?
C29 C30 N7 108.7(3) . . ?
C29 C30 N9 139.9(4) . . ?
N7 C30 N9 111.4(3) . . ?
N8 C31 C29 114.6(4) . . ?
N8 C31 H31 122.7 . . ?
C29 C31 H31 122.7 . . ?
N9 C32 C42 120.8(4) . . ?
N9 C32 C33 112.3(3) . . ?
C42 C32 C33 126.9(4) . . ?
N10 C33 N7 135.9(4) . . ?
N10 C33 C32 123.7(4) . . ?
N7 C33 C32 100.4(3) . . ?
N10 C34 C37 109.0(4) . . ?
N10 C34 C38 103.9(3) . . ?
C37 C34 C38 108.5(4) . . ?
N10 C34 C35 113.2(3) . . ?
C37 C34 C35 108.0(4) . . ?
C38 C34 C35 114.0(4) . . ?
C36 C35 C34 123.9(4) . . ?
C36 C35 H35A 106.4 . . ?
C34 C35 H35A 106.4 . . ?
C36 C35 H35B 106.4 . . ?
C34 C35 H35B 106.4 . . ?
H35A C35 H35B 106.4 . . ?
C39 C36 C40 109.8(5) . . ?
C39 C36 C35 111.9(4) . . ?
C40 C36 C35 113.1(4) . . ?
C39 C36 C41 109.6(5) . . ?
C40 C36 C41 106.4(5) . . ?
C35 C36 C41 105.8(4) . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C36 C40 H40A 109.5 . . ?
C36 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C36 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C36 C41 H41A 109.5 . . ?
C36 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C36 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C47 117.1(4) . . ?
C43 C42 C32 118.4(4) . . ?
C47 C42 C32 124.5(4) . . ?
C44 C43 C42 122.6(4) . . ?
C44 C43 H43 118.7 . . ?
C42 C43 H43 118.7 . . ?
C43 C44 C45 119.4(4) . . ?
C43 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
N11 C45 C44 125.2(4) . . ?
N11 C45 C46 115.4(4) . . ?
C44 C45 C46 119.4(4) . . ?
C47 C46 C45 119.9(4) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C46 C47 C42 121.5(4) . . ?
C46 C47 H47 119.2 . . ?
C42 C47 H47 119.2 . . ?
N11 C48 H48A 109.5 . . ?
N11 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N11 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C5 N1 C8 118.1(3) . . ?
N3 N2 C10 112.1(3) . . ?
N3 N2 C13 138.4(3) . . ?
C10 N2 C13 109.1(3) . . ?
C11 N3 N2 103.2(3) . . ?
C12 N4 C10 106.4(3) . . ?
C13 N5 C14 127.5(3) . . ?
C25 N6 C28 117.7(4) . . ?
C30 N7 N8 112.4(3) . . ?
C30 N7 C33 109.3(3) . . ?
N8 N7 C33 138.1(3) . . ?
C31 N8 N7 102.4(3) . . ?
C32 N9 C30 106.5(3) . . ?
C33 N10 C34 127.4(4) . . ?
C45 N11 C48 116.7(3) . . ?
Cl2 C49 Cl1 114.3(6) . . ?
Cl2 C49 H49A 108.7 . . ?
Cl1 C49 H49A 108.7 . . ?
Cl2 C49 H49B 108.7 . . ?
Cl1 C49 H49B 108.7 . . ?
H49A C49 H49B 107.6 . . ?

_refine_diff_density_max         1.043
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_md164-1-e_170k
_database_code_depnum_ccdc_archive 'CCDC 1812146'
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H62 N11'
_chemical_formula_weight         817.10

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'

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

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

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

_cell_length_a                   24.6041(16)
_cell_length_b                   6.0490(7)
_cell_length_c                   31.305(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.106(6)
_cell_angle_gamma                90
_cell_volume                     4656.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    3206
_cell_measurement_theta_min      3.7930
_cell_measurement_theta_max      26.9630

_exptl_crystal_description       'prism (fragment of)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_F_000             1756
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 0 0 0.0250 0.9940 0.0001 0.0007 -0.0010 -0.0271 0.0093
9 -1 -19 0.0650 8.8750 -0.9934 -18.8674 0.4306 -0.2608 0.0273
4 0 1 0.0350 3.9779 0.0003 0.9940 -0.0263 -0.1095 0.0344
16 1 6 0.0500 15.9092 0.9934 5.9840 -0.1661 -0.4019 0.2406
-6 1 12 0.0850 -5.9228 0.9929 11.9250 -0.2776 0.1873 0.0199
0 -1 14 0.0850 0.0669 -0.9905 13.8636 -0.2960 -0.0538 -0.1474
2 1 6 0.1000 2.0007 0.9927 5.9771 -0.1519 -0.0227 0.1107
1 0 -2 0.0500 0.9854 -0.0002 -1.9835 0.0436 -0.0249 0.0148
-10 -1 17 0.0600 -9.8556 -0.9907 16.8346 -0.3527 0.2137 -0.2485
-1 0 2 0.0550 -0.9854 0.0002 1.9835 -0.0436 0.0249 -0.0148
-3 0 2 0.0450 -2.9723 0.0000 1.9825 -0.0416 0.0790 -0.0334
-1 0 0 0.0450 -0.9940 -0.0001 -0.0007 0.0010 0.0271 -0.0093
0 0 -1 0.0600 -0.0037 -0.0001 -0.9917 0.0223 0.0011 0.0028
0 -1 0 0.1700 0.0104 -0.9919 -0.0242 0.0162 -0.0382 -0.1087
0 1 0 0.1700 -0.0104 0.9919 0.0242 -0.0162 0.0382 0.1087

_exptl_absorpt_coefficient_mu    0.071
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_reflns_number            19938
_diffrn_reflns_av_unetI/netI     0.1254
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.330
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_orient_matrix_UB_11      -0.0010063000
_diffrn_orient_matrix_UB_12      -0.0157452000
_diffrn_orient_matrix_UB_13      -0.0224682000
_diffrn_orient_matrix_UB_21      -0.0272654000
_diffrn_orient_matrix_UB_22      0.0382398000
_diffrn_orient_matrix_UB_23      -0.0010171000
_diffrn_orient_matrix_UB_31      0.0093361000
_diffrn_orient_matrix_UB_32      0.1097911000
_diffrn_orient_matrix_UB_33      -0.0028355000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -8.00   49.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7155   77.0000  -90.0000 57

#__ type_ start__ end____ width___ exp.time_
  2 omega   22.00   86.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6530   77.0000 -150.0000 64

#__ type_ start__ end____ width___ exp.time_
  3 omega  -16.00  106.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6530   77.0000  150.0000 122

;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             9527
_reflns_number_gt                4834
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;

_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;

_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;

_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
WinGX Version 2014.12, J.L. Farrugia, 212, J Appl. Cryst. 45, 849-854
;
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0770P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9527
_refine_ls_number_parameters     566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.2154
_refine_ls_wR_factor_gt          0.1666
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.42762(11) 0.5172(6) 0.29338(9) 0.0422(8) Uani 1 1 d . . . . .
H1 H 0.4303 0.6816 0.2961 0.051 Uiso 1 1 calc R U . . .
C2 C 0.39896(11) 0.4330(6) 0.33245(10) 0.0440(8) Uani 1 1 d . . . . .
C3 C 0.36968(12) 0.2358(7) 0.33163(11) 0.0537(9) Uani 1 1 d . . . . .
H3 H 0.3652 0.1558 0.3056 0.064 Uiso 1 1 calc R U . . .
C4 C 0.34716(13) 0.1560(7) 0.36807(11) 0.0587(10) Uani 1 1 d . . . . .
H4 H 0.3269 0.0222 0.3667 0.070 Uiso 1 1 calc R U . . .
C5 C 0.35327(12) 0.2659(7) 0.40659(11) 0.0523(9) Uani 1 1 d . . . . .
C6 C 0.38193(12) 0.4641(7) 0.40788(10) 0.0518(9) Uani 1 1 d . . . . .
H6 H 0.3865 0.5438 0.4339 0.062 Uiso 1 1 calc R U . . .
C7 C 0.40395(12) 0.5449(6) 0.37034(10) 0.0491(9) Uani 1 1 d . . . . .
H7 H 0.4229 0.6816 0.3712 0.059 Uiso 1 1 calc R U . . .
C8 C 0.33081(14) 0.2923(8) 0.47921(12) 0.0698(12) Uani 1 1 d . . . . .
H8A H 0.3685 0.3074 0.4899 0.105 Uiso 1 1 calc R U . . .
H8B H 0.3096 0.2154 0.5005 0.105 Uiso 1 1 calc R U . . .
H8C H 0.3153 0.4393 0.4738 0.105 Uiso 1 1 calc R U . . .
C9I C 0.39676(11) 0.4686(6) 0.25194(10) 0.0448(8) Uani 1 1 d . . . . .
C9J C 0.48514(11) 0.4288(6) 0.29231(9) 0.0391(7) Uani 1 1 d . . . . .
C10I C 0.41066(11) 0.3381(6) 0.21834(10) 0.0453(8) Uani 1 1 d . . . . .
C10J C 0.50912(11) 0.2542(6) 0.31323(9) 0.0390(8) Uani 1 1 d . . . . .
C11I C 0.34415(12) 0.5507(7) 0.23859(10) 0.0503(9) Uani 1 1 d . . . . .
C11J C 0.52718(12) 0.5135(6) 0.26638(9) 0.0439(8) Uani 1 1 d . . . . .
C12I C 0.43785(11) 0.1232(6) 0.16850(10) 0.0421(8) Uani 1 1 d . . . . .
C12J C 0.54395(10) -0.0169(6) 0.34973(9) 0.0383(8) Uani 1 1 d . . . . .
C13I C 0.38210(11) 0.2077(6) 0.15318(9) 0.0400(8) Uani 1 1 d . . . . .
C13J C 0.58909(11) 0.0701(5) 0.32288(9) 0.0360(7) Uani 1 1 d . . . . .
C14I C 0.30700(11) 0.2399(6) 0.10027(10) 0.0420(8) Uani 1 1 d . . . . .
C14J C 0.68307(11) 0.0763(6) 0.30042(9) 0.0385(7) Uani 1 1 d . . . . .
C15I C 0.29779(12) 0.1373(6) 0.05570(9) 0.0458(8) Uani 1 1 d . . . . .
H15A H 0.2599 0.1744 0.0466 0.055 Uiso 1 1 calc R U . . .
H15B H 0.2987 -0.0249 0.0600 0.055 Uiso 1 1 calc R U . . .
C15J C 0.73382(11) -0.0602(6) 0.31401(9) 0.0413(8) Uani 1 1 d . . . . .
H15C H 0.7242 -0.2170 0.3087 0.050 Uiso 1 1 calc R U . . .
H15D H 0.7621 -0.0225 0.2936 0.050 Uiso 1 1 calc R U . . .
C16I C 0.33261(13) 0.1836(7) 0.01692(10) 0.0525(9) Uani 1 1 d . . . . .
C16J C 0.76177(11) -0.0518(6) 0.35882(10) 0.0442(8) Uani 1 1 d . . . . .
C17I C 0.26316(11) 0.1470(7) 0.12916(11) 0.0539(10) Uani 1 1 d . . . . .
H17A H 0.2671 -0.0138 0.1313 0.081 Uiso 1 1 calc R U . . .
H17B H 0.2270 0.1828 0.1168 0.081 Uiso 1 1 calc R U . . .
H17C H 0.2674 0.2130 0.1577 0.081 Uiso 1 1 calc R U . . .
C17J C 0.66988(12) 0.0220(7) 0.25296(9) 0.0510(9) Uani 1 1 d . . . . .
H17D H 0.6633 -0.1370 0.2498 0.077 Uiso 1 1 calc R U . . .
H17E H 0.7006 0.0649 0.2358 0.077 Uiso 1 1 calc R U . . .
H17F H 0.6374 0.1037 0.2432 0.077 Uiso 1 1 calc R U . . .
C18I C 0.30460(12) 0.4923(6) 0.09977(11) 0.0501(9) Uani 1 1 d . . . . .
H18A H 0.3012 0.5472 0.1290 0.075 Uiso 1 1 calc R U . . .
H18B H 0.2731 0.5406 0.0821 0.075 Uiso 1 1 calc R U . . .
H18C H 0.3379 0.5510 0.0879 0.075 Uiso 1 1 calc R U . . .
C18J C 0.69200(11) 0.3249(6) 0.30593(11) 0.0475(8) Uani 1 1 d . . . . .
H18D H 0.6631 0.4054 0.2901 0.071 Uiso 1 1 calc R U . . .
H18E H 0.7274 0.3657 0.2948 0.071 Uiso 1 1 calc R U . . .
H18F H 0.6913 0.3631 0.3363 0.071 Uiso 1 1 calc R U . . .
C19I C 0.32804(18) 0.4224(8) 0.00141(13) 0.0802(13) Uani 1 1 d . . . . .
H19A H 0.2896 0.4632 -0.0021 0.120 Uiso 1 1 calc R U . . .
H19B H 0.3456 0.4368 -0.0261 0.120 Uiso 1 1 calc R U . . .
H19C H 0.3460 0.5205 0.0224 0.120 Uiso 1 1 calc R U . . .
C19J C 0.72432(14) -0.1232(10) 0.39366(11) 0.0829(16) Uani 1 1 d . . . . .
H19D H 0.7450 -0.1323 0.4210 0.124 Uiso 1 1 calc R U . . .
H19E H 0.7088 -0.2685 0.3865 0.124 Uiso 1 1 calc R U . . .
H19F H 0.6949 -0.0151 0.3960 0.124 Uiso 1 1 calc R U . . .
C20I C 0.39248(14) 0.1237(10) 0.02540(12) 0.0849(16) Uani 1 1 d . . . . .
H20A H 0.4081 0.2203 0.0478 0.127 Uiso 1 1 calc R U . . .
H20B H 0.4124 0.1430 -0.0009 0.127 Uiso 1 1 calc R U . . .
H20C H 0.3952 -0.0307 0.0348 0.127 Uiso 1 1 calc R U . . .
C20J C 0.80961(13) -0.2159(7) 0.35782(12) 0.0663(11) Uani 1 1 d . . . . .
H20D H 0.8368 -0.1609 0.3383 0.099 Uiso 1 1 calc R U . . .
H20E H 0.7963 -0.3603 0.3479 0.099 Uiso 1 1 calc R U . . .
H20F H 0.8262 -0.2310 0.3866 0.099 Uiso 1 1 calc R U . . .
C21I C 0.31053(16) 0.0392(7) -0.01973(11) 0.0696(11) Uani 1 1 d . . . . .
H21A H 0.3114 -0.1162 -0.0109 0.104 Uiso 1 1 calc R U . . .
H21B H 0.3331 0.0586 -0.0446 0.104 Uiso 1 1 calc R U . . .
H21C H 0.2730 0.0825 -0.0272 0.104 Uiso 1 1 calc R U . . .
C21J C 0.78676(15) 0.1731(7) 0.36963(13) 0.0739(12) Uani 1 1 d . . . . .
H21D H 0.7579 0.2776 0.3764 0.111 Uiso 1 1 calc R U . . .
H21E H 0.8064 0.2277 0.3451 0.111 Uiso 1 1 calc R U . . .
H21F H 0.8121 0.1583 0.3944 0.111 Uiso 1 1 calc R U . . .
C22I C 0.47064(11) -0.0275(6) 0.14396(9) 0.0425(8) Uani 1 1 d . . . . .
C22J C 0.55042(11) -0.1938(6) 0.38095(9) 0.0387(8) Uani 1 1 d . . . . .
C23I C 0.52701(11) -0.0082(6) 0.14554(10) 0.0481(9) Uani 1 1 d . . . . .
H23I H 0.5437 0.1076 0.1618 0.058 Uiso 1 1 calc R U . . .
C23J C 0.51988(11) -0.1920(6) 0.41773(10) 0.0478(9) Uani 1 1 d . . . . .
H23J H 0.4937 -0.0787 0.4213 0.057 Uiso 1 1 calc R U . . .
C24I C 0.55913(13) -0.1547(7) 0.12384(11) 0.0556(10) Uani 1 1 d . . . . .
H24I H 0.5976 -0.1382 0.1250 0.067 Uiso 1 1 calc R U . . .
C24J C 0.52692(12) -0.3503(7) 0.44866(10) 0.0533(10) Uani 1 1 d . . . . .
H24J H 0.5060 -0.3443 0.4736 0.064 Uiso 1 1 calc R U . . .
C25I C 0.53528(13) -0.3265(7) 0.10029(10) 0.0536(10) Uani 1 1 d . . . . .
C25J C 0.56457(12) -0.5206(6) 0.44398(10) 0.0480(9) Uani 1 1 d . . . . .
C26I C 0.47905(13) -0.3506(7) 0.09879(11) 0.0593(10) Uani 1 1 d . . . . .
H26I H 0.4624 -0.4692 0.0833 0.071 Uiso 1 1 calc R U . . .
C26J C 0.59442(12) -0.5291(6) 0.40709(10) 0.0467(8) Uani 1 1 d . . . . .
H26J H 0.6197 -0.6455 0.4031 0.056 Uiso 1 1 calc R U . . .
C27I C 0.44750(13) -0.1997(7) 0.12017(11) 0.0554(10) Uani 1 1 d . . . . .
H27I H 0.4090 -0.2143 0.1185 0.066 Uiso 1 1 calc R U . . .
C27J C 0.58718(11) -0.3674(6) 0.37625(10) 0.0441(8) Uani 1 1 d . . . . .
H27J H 0.6077 -0.3743 0.3512 0.053 Uiso 1 1 calc R U . . .
C28I C 0.54792(16) -0.6356(8) 0.05557(13) 0.0781(13) Uani 1 1 d . . . . .
H28A H 0.5245 -0.7265 0.0731 0.117 Uiso 1 1 calc R U . . .
H28B H 0.5773 -0.7270 0.0448 0.117 Uiso 1 1 calc R U . . .
H28C H 0.5264 -0.5738 0.0315 0.117 Uiso 1 1 calc R U . . .
C28J C 0.61181(16) -0.8263(7) 0.47605(12) 0.0674(11) Uani 1 1 d . . . . .
H28D H 0.6051 -0.9261 0.4518 0.101 Uiso 1 1 calc R U . . .
H28E H 0.6126 -0.9115 0.5027 0.101 Uiso 1 1 calc R U . . .
H28F H 0.6468 -0.7517 0.4731 0.101 Uiso 1 1 calc R U . . .
C29I C 0.30955(14) 0.7078(8) 0.26226(11) 0.0706(13) Uani 1 1 d . . . . .
H29A H 0.3279 0.8512 0.2647 0.106 Uiso 1 1 calc R U . . .
H29B H 0.3035 0.6493 0.2909 0.106 Uiso 1 1 calc R U . . .
H29C H 0.2745 0.7262 0.2467 0.106 Uiso 1 1 calc R U . . .
C29J C 0.52334(13) 0.7029(7) 0.23621(11) 0.0556(10) Uani 1 1 d . . . . .
H29D H 0.5598 0.7423 0.2272 0.083 Uiso 1 1 calc R U . . .
H29E H 0.5071 0.8298 0.2504 0.083 Uiso 1 1 calc R U . . .
H29F H 0.5006 0.6615 0.2111 0.083 Uiso 1 1 calc R U . . .
N1 N 0.32945(9) 0.1700(5) 0.44097(7) 0.0435(7) Uani 1 1 d . . . . .
N2I N 0.36929(9) 0.3403(5) 0.18830(8) 0.0457(7) Uani 1 1 d . . . . .
N2J N 0.49824(9) 0.0920(5) 0.34394(7) 0.0415(7) Uani 1 1 d . . . . .
N3I N 0.32699(9) 0.4761(5) 0.20071(8) 0.0520(8) Uani 1 1 d . . . . .
N3J N 0.56144(9) 0.2387(5) 0.30001(7) 0.0399(6) Uani 1 1 d . . . . .
N4I N 0.45352(9) 0.2007(5) 0.20555(8) 0.0446(7) Uani 1 1 d . . . . .
N4J N 0.57356(9) 0.3994(5) 0.27083(8) 0.0448(7) Uani 1 1 d . . . . .
N5I N 0.36050(9) 0.1610(5) 0.11712(8) 0.0413(7) Uani 1 1 d . . . . .
N5J N 0.63738(9) -0.0034(5) 0.32544(7) 0.0393(6) Uani 1 1 d . . . . .
N6I N 0.57028(9) -0.4627(5) 0.08048(8) 0.0468(7) Uani 1 1 d . . . . .
N6J N 0.56955(9) -0.6657(5) 0.47697(8) 0.0434(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C9I 1.508(4) . ?
C1 C9J 1.514(4) . ?
C1 C2 1.522(4) . ?
C1 H1 1.0000 . ?
C2 C7 1.367(4) . ?
C2 C3 1.393(5) . ?
C3 C4 1.374(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(5) . ?
C4 H4 0.9500 . ?
C5 N1 1.373(4) . ?
C5 C6 1.391(5) . ?
C6 C7 1.400(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 N1 1.407(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9I C10I 1.368(4) . ?
C9I C11I 1.434(4) . ?
C9J C10J 1.365(4) . ?
C9J C11J 1.433(4) . ?
C10I N2I 1.360(3) . ?
C10I N4I 1.412(4) . ?
C10J N3J 1.370(3) . ?
C10J N2J 1.406(4) . ?
C11I N3I 1.324(4) . ?
C11I C29I 1.491(5) . ?
C11J N4J 1.336(4) . ?
C11J C29J 1.486(5) . ?
C12I N4I 1.296(4) . ?
C12I C22I 1.455(4) . ?
C12I C13I 1.525(4) . ?
C12J N2J 1.310(4) . ?
C12J C22J 1.454(4) . ?
C12J C13J 1.512(4) . ?
C13I N5I 1.262(3) . ?
C13I N2I 1.406(4) . ?
C13J N5J 1.268(3) . ?
C13J N3J 1.407(4) . ?
C14I N5I 1.479(3) . ?
C14I C18I 1.528(5) . ?
C14I C15I 1.536(4) . ?
C14I C17I 1.539(4) . ?
C14J N5J 1.474(3) . ?
C14J C18J 1.529(5) . ?
C14J C15J 1.544(4) . ?
C14J C17J 1.544(4) . ?
C15I C16I 1.537(4) . ?
C15I H15A 0.9900 . ?
C15I H15B 0.9900 . ?
C15J C16J 1.540(4) . ?
C15J H15C 0.9900 . ?
C15J H15D 0.9900 . ?
C16I C21I 1.526(5) . ?
C16I C19I 1.527(6) . ?
C16I C20I 1.531(5) . ?
C16J C19J 1.516(4) . ?
C16J C21J 1.526(5) . ?
C16J C20J 1.541(4) . ?
C17I H17A 0.9800 . ?
C17I H17B 0.9800 . ?
C17I H17C 0.9800 . ?
C17J H17D 0.9800 . ?
C17J H17E 0.9800 . ?
C17J H17F 0.9800 . ?
C18I H18A 0.9800 . ?
C18I H18B 0.9800 . ?
C18I H18C 0.9800 . ?
C18J H18D 0.9800 . ?
C18J H18E 0.9800 . ?
C18J H18F 0.9800 . ?
C19I H19A 0.9800 . ?
C19I H19B 0.9800 . ?
C19I H19C 0.9800 . ?
C19J H19D 0.9800 . ?
C19J H19E 0.9800 . ?
C19J H19F 0.9800 . ?
C20I H20A 0.9800 . ?
C20I H20B 0.9800 . ?
C20I H20C 0.9800 . ?
C20J H20D 0.9800 . ?
C20J H20E 0.9800 . ?
C20J H20F 0.9800 . ?
C21I H21A 0.9800 . ?
C21I H21B 0.9800 . ?
C21I H21C 0.9800 . ?
C21J H21D 0.9800 . ?
C21J H21E 0.9800 . ?
C21J H21F 0.9800 . ?
C22I C27I 1.390(5) . ?
C22I C23I 1.391(4) . ?
C22J C27J 1.397(4) . ?
C22J C23J 1.398(4) . ?
C23I C24I 1.383(5) . ?
C23I H23I 0.9500 . ?
C23J C24J 1.368(5) . ?
C23J H23J 0.9500 . ?
C24I C25I 1.391(5) . ?
C24I H24I 0.9500 . ?
C24J C25J 1.397(5) . ?
C24J H24J 0.9500 . ?
C25I N6I 1.358(4) . ?
C25I C26I 1.390(4) . ?
C25J N6J 1.357(4) . ?
C25J C26J 1.392(4) . ?
C26I C27I 1.386(5) . ?
C26I H26I 0.9500 . ?
C26J C27J 1.381(4) . ?
C26J H26J 0.9500 . ?
C27I H27I 0.9500 . ?
C27J H27J 0.9500 . ?
C28I N6I 1.404(5) . ?
C28I H28A 0.9800 . ?
C28I H28B 0.9800 . ?
C28I H28C 0.9800 . ?
C28J N6J 1.424(4) . ?
C28J H28D 0.9800 . ?
C28J H28E 0.9800 . ?
C28J H28F 0.9800 . ?
C29I H29A 0.9800 . ?
C29I H29B 0.9800 . ?
C29I H29C 0.9800 . ?
C29J H29D 0.9800 . ?
C29J H29E 0.9800 . ?
C29J H29F 0.9800 . ?
N2I N3I 1.392(3) . ?
N3J N4J 1.374(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9I C1 C9J 110.7(2) . . ?
C9I C1 C2 113.1(3) . . ?
C9J C1 C2 111.1(3) . . ?
C9I C1 H1 107.2 . . ?
C9J C1 H1 107.2 . . ?
C2 C1 H1 107.2 . . ?
C7 C2 C3 118.0(3) . . ?
C7 C2 C1 120.1(3) . . ?
C3 C2 C1 121.7(3) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 121.4(4) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
N1 C5 C4 116.5(3) . . ?
N1 C5 C6 124.9(3) . . ?
C4 C5 C6 118.7(3) . . ?
C5 C6 C7 119.2(3) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C2 C7 C6 122.0(3) . . ?
C2 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10I C9I C11I 103.0(3) . . ?
C10I C9I C1 129.9(3) . . ?
C11I C9I C1 127.1(3) . . ?
C10J C9J C11J 103.9(3) . . ?
C10J C9J C1 130.6(3) . . ?
C11J C9J C1 125.5(3) . . ?
N2I C10I C9I 108.9(3) . . ?
N2I C10I N4I 110.9(3) . . ?
C9I C10I N4I 140.2(3) . . ?
C9J C10J N3J 107.6(3) . . ?
C9J C10J N2J 141.1(3) . . ?
N3J C10J N2J 111.3(3) . . ?
N3I C11I C9I 113.4(3) . . ?
N3I C11I C29I 119.6(3) . . ?
C9I C11I C29I 127.0(3) . . ?
N4J C11J C9J 112.8(3) . . ?
N4J C11J C29J 119.9(3) . . ?
C9J C11J C29J 127.3(3) . . ?
N4I C12I C22I 123.1(3) . . ?
N4I C12I C13I 113.2(3) . . ?
C22I C12I C13I 123.6(3) . . ?
N2J C12J C22J 122.4(2) . . ?
N2J C12J C13J 113.1(3) . . ?
C22J C12J C13J 124.4(3) . . ?
N5I C13I N2I 136.7(3) . . ?
N5I C13I C12I 123.4(3) . . ?
N2I C13I C12I 99.8(2) . . ?
N5J C13J N3J 136.1(3) . . ?
N5J C13J C12J 123.3(3) . . ?
N3J C13J C12J 100.6(2) . . ?
N5I C14I C18I 111.1(2) . . ?
N5I C14I C15I 107.0(2) . . ?
C18I C14I C15I 113.0(3) . . ?
N5I C14I C17I 107.8(3) . . ?
C18I C14I C17I 110.1(3) . . ?
C15I C14I C17I 107.6(3) . . ?
N5J C14J C18J 111.8(2) . . ?
N5J C14J C15J 107.7(2) . . ?
C18J C14J C15J 112.6(2) . . ?
N5J C14J C17J 107.7(2) . . ?
C18J C14J C17J 110.0(3) . . ?
C15J C14J C17J 106.9(2) . . ?
C14I C15I C16I 125.1(3) . . ?
C14I C15I H15A 106.0 . . ?
C16I C15I H15A 106.0 . . ?
C14I C15I H15B 106.0 . . ?
C16I C15I H15B 106.0 . . ?
H15A C15I H15B 106.3 . . ?
C16J C15J C14J 124.3(3) . . ?
C16J C15J H15C 106.3 . . ?
C14J C15J H15C 106.3 . . ?
C16J C15J H15D 106.3 . . ?
C14J C15J H15D 106.3 . . ?
H15C C15J H15D 106.4 . . ?
C21I C16I C19I 106.4(3) . . ?
C21I C16I C20I 108.0(3) . . ?
C19I C16I C20I 109.8(3) . . ?
C21I C16I C15I 107.2(3) . . ?
C19I C16I C15I 112.8(3) . . ?
C20I C16I C15I 112.4(3) . . ?
C19J C16J C21J 110.2(3) . . ?
C19J C16J C15J 112.5(3) . . ?
C21J C16J C15J 113.2(3) . . ?
C19J C16J C20J 108.4(3) . . ?
C21J C16J C20J 106.1(3) . . ?
C15J C16J C20J 106.0(3) . . ?
C14I C17I H17A 109.5 . . ?
C14I C17I H17B 109.5 . . ?
H17A C17I H17B 109.5 . . ?
C14I C17I H17C 109.5 . . ?
H17A C17I H17C 109.5 . . ?
H17B C17I H17C 109.5 . . ?
C14J C17J H17D 109.5 . . ?
C14J C17J H17E 109.5 . . ?
H17D C17J H17E 109.5 . . ?
C14J C17J H17F 109.5 . . ?
H17D C17J H17F 109.5 . . ?
H17E C17J H17F 109.5 . . ?
C14I C18I H18A 109.5 . . ?
C14I C18I H18B 109.5 . . ?
H18A C18I H18B 109.5 . . ?
C14I C18I H18C 109.5 . . ?
H18A C18I H18C 109.5 . . ?
H18B C18I H18C 109.5 . . ?
C14J C18J H18D 109.5 . . ?
C14J C18J H18E 109.5 . . ?
H18D C18J H18E 109.5 . . ?
C14J C18J H18F 109.5 . . ?
H18D C18J H18F 109.5 . . ?
H18E C18J H18F 109.5 . . ?
C16I C19I H19A 109.5 . . ?
C16I C19I H19B 109.5 . . ?
H19A C19I H19B 109.5 . . ?
C16I C19I H19C 109.5 . . ?
H19A C19I H19C 109.5 . . ?
H19B C19I H19C 109.5 . . ?
C16J C19J H19D 109.5 . . ?
C16J C19J H19E 109.5 . . ?
H19D C19J H19E 109.5 . . ?
C16J C19J H19F 109.5 . . ?
H19D C19J H19F 109.5 . . ?
H19E C19J H19F 109.5 . . ?
C16I C20I H20A 109.5 . . ?
C16I C20I H20B 109.5 . . ?
H20A C20I H20B 109.5 . . ?
C16I C20I H20C 109.5 . . ?
H20A C20I H20C 109.5 . . ?
H20B C20I H20C 109.5 . . ?
C16J C20J H20D 109.5 . . ?
C16J C20J H20E 109.5 . . ?
H20D C20J H20E 109.5 . . ?
C16J C20J H20F 109.5 . . ?
H20D C20J H20F 109.5 . . ?
H20E C20J H20F 109.5 . . ?
C16I C21I H21A 109.5 . . ?
C16I C21I H21B 109.5 . . ?
H21A C21I H21B 109.5 . . ?
C16I C21I H21C 109.5 . . ?
H21A C21I H21C 109.5 . . ?
H21B C21I H21C 109.5 . . ?
C16J C21J H21D 109.5 . . ?
C16J C21J H21E 109.5 . . ?
H21D C21J H21E 109.5 . . ?
C16J C21J H21F 109.5 . . ?
H21D C21J H21F 109.5 . . ?
H21E C21J H21F 109.5 . . ?
C27I C22I C23I 118.0(3) . . ?
C27I C22I C12I 121.9(3) . . ?
C23I C22I C12I 120.0(3) . . ?
C27J C22J C23J 117.5(3) . . ?
C27J C22J C12J 122.5(3) . . ?
C23J C22J C12J 119.9(3) . . ?
C24I C23I C22I 121.1(3) . . ?
C24I C23I H23I 119.5 . . ?
C22I C23I H23I 119.5 . . ?
C24J C23J C22J 121.3(3) . . ?
C24J C23J H23J 119.3 . . ?
C22J C23J H23J 119.3 . . ?
C23I C24I C25I 120.1(3) . . ?
C23I C24I H24I 119.9 . . ?
C25I C24I H24I 119.9 . . ?
C23J C24J C25J 120.6(3) . . ?
C23J C24J H24J 119.7 . . ?
C25J C24J H24J 119.7 . . ?
N6I C25I C26I 124.6(4) . . ?
N6I C25I C24I 115.7(3) . . ?
C26I C25I C24I 119.8(3) . . ?
N6J C25J C26J 124.9(3) . . ?
N6J C25J C24J 116.0(3) . . ?
C26J C25J C24J 119.1(3) . . ?
C27I C26I C25I 119.2(4) . . ?
C27I C26I H26I 120.4 . . ?
C25I C26I H26I 120.4 . . ?
C27J C26J C25J 119.7(3) . . ?
C27J C26J H26J 120.2 . . ?
C25J C26J H26J 120.2 . . ?
C26I C27I C22I 121.8(3) . . ?
C26I C27I H27I 119.1 . . ?
C22I C27I H27I 119.1 . . ?
C26J C27J C22J 121.7(3) . . ?
C26J C27J H27J 119.1 . . ?
C22J C27J H27J 119.1 . . ?
N6I C28I H28A 109.5 . . ?
N6I C28I H28B 109.5 . . ?
H28A C28I H28B 109.5 . . ?
N6I C28I H28C 109.5 . . ?
H28A C28I H28C 109.5 . . ?
H28B C28I H28C 109.5 . . ?
N6J C28J H28D 109.5 . . ?
N6J C28J H28E 109.5 . . ?
H28D C28J H28E 109.5 . . ?
N6J C28J H28F 109.5 . . ?
H28D C28J H28F 109.5 . . ?
H28E C28J H28F 109.5 . . ?
C11I C29I H29A 109.5 . . ?
C11I C29I H29B 109.5 . . ?
H29A C29I H29B 109.5 . . ?
C11I C29I H29C 109.5 . . ?
H29A C29I H29C 109.5 . . ?
H29B C29I H29C 109.5 . . ?
C11J C29J H29D 109.5 . . ?
C11J C29J H29E 109.5 . . ?
H29D C29J H29E 109.5 . . ?
C11J C29J H29F 109.5 . . ?
H29D C29J H29F 109.5 . . ?
H29E C29J H29F 109.5 . . ?
C5 N1 C8 116.6(3) . . ?
C10I N2I N3I 111.1(2) . . ?
C10I N2I C13I 110.6(2) . . ?
N3I N2I C13I 138.3(2) . . ?
C12J N2J C10J 105.2(2) . . ?
C11I N3I N2I 103.5(2) . . ?
C10J N3J N4J 112.5(2) . . ?
C10J N3J C13J 109.7(2) . . ?
N4J N3J C13J 137.6(2) . . ?
C12I N4I C10I 105.4(2) . . ?
C11J N4J N3J 103.3(2) . . ?
C13I N5I C14I 125.9(3) . . ?
C13J N5J C14J 125.6(3) . . ?
C25I N6I C28I 117.6(3) . . ?
C25J N6J C28J 118.1(3) . . ?

_refine_diff_density_max         0.354
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.052

