# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_compound_3b
_database_code_depnum_ccdc_archive 'CCDC 1559108'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;


_audit_creation_date             2017-01-24
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H43 N2, Br'
_chemical_formula_sum            'C34 H43 Br N2'
_chemical_formula_weight         559.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H43 Br N2'
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'
Br Br -0.6763 1.2805 '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'

_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                   12.65346(19)
_cell_length_b                   15.1670(2)
_cell_length_c                   18.3140(3)
_cell_angle_alpha                110.1753(14)
_cell_angle_beta                 102.3785(13)
_cell_angle_gamma                96.7444(12)
_cell_volume                     3151.39(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27833
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2620
_cell_measurement_theta_min      3.1400
_exptl_absorpt_coefficient_mu    1.933
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0116
-5 -2 2 0.0524
5 2 -2 0.0524
5 -5 1 0.0329
-5 5 -1 0.0329
0 0 -1 0.0116

_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.023
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0005 -0.0011 0.9997 0.0876 0.0298 0.0099
-4.9957 -1.9961 1.9908 -0.2456 0.5773 -0.2406
4.9957 1.9961 -1.9908 0.2456 -0.5773 0.2406
4.9976 -4.9994 0.9957 0.0171 -0.1212 0.7426
-4.9976 4.9994 -0.9957 -0.0171 0.1212 -0.7426
0.0005 0.0011 -0.9997 -0.0876 -0.0298 -0.0099

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61446
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.55
_diffrn_reflns_theta_min         2.67
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  30.00   1.00    3.50    --  -38.50  77.00 -30.00   98
  2  ω   -105.00  -6.00   1.00    3.50    --  -38.50 -19.00 -30.00   99
  3  ω    -58.00  33.00   1.00    3.50    --  -38.50  38.00  90.00   91
  4  ω   -109.00 -18.00   1.00    3.50    --  -38.50 -38.00 -90.00   91
  5  ω      2.00  79.00   1.00    3.50    --   43.45 -99.00 150.00   77
  6  ω     13.00  89.00   1.00    3.50    --   43.45  77.00-180.00   76
  7  ω     13.00  64.00   1.00    3.50    --   43.45  77.00   0.00   51
  8  ω     13.00  76.00   1.00    3.50    --   43.45  77.00 -90.00   63
  9  ω     18.00  44.00   1.00    3.50    --   43.45  57.00-150.00   26
 10  ω     14.00 110.00   1.00    3.50    --   43.45  77.00  90.00   96
 11  ω     61.00  92.00   1.00    3.50    --   43.45  57.00-150.00   31
 12  ω     18.00  83.00   1.00    3.50    --   43.45  57.00  60.00   65
 13  ω     58.00 108.00   1.00    3.50    --   43.45 178.00 -30.00   50
 14  ω     81.00 178.00   1.00   14.00    --  111.00  77.00-150.00   97
 15  ω     85.00 170.00   1.00   14.00    --  111.00  61.00 120.00   85
 16  ω     88.00 167.00   1.00   14.00    --  111.00  49.00 -93.44   79
 17  ω     45.00 106.00   1.00   14.00    --  111.00 -77.00-180.00   61
 18  ω     81.00 107.00   1.00   14.00    --  111.00  77.00 -30.00   26
 19  ω     83.00 109.00   1.00   14.00    --  111.00  70.00  -7.86   26
 20  ω     84.00 177.00   1.00   14.00    --  111.00  63.00 155.69   93
 21  ω     85.00 111.00   1.00   14.00    --  111.00  61.00  60.00   26
 22  ω     41.00 122.00   1.00   14.00    --  111.00-125.00-150.00   81
 23  ω     82.00 107.00   1.00   14.00    --  111.00  77.00-120.00   25
 24  ω     81.00 107.00   1.00   14.00    --  111.00  77.00 120.00   26
 25  ω     44.00 134.00   1.00   14.00    --  111.00 -61.00  30.00   90
 26  ω     85.00 111.00   1.00   14.00    --  111.00  61.00-180.00   26
 27  ω     85.00 177.00   1.00   14.00    --  111.00  61.00 -30.00   92
 28  ω     85.00 163.00   1.00   14.00    --  111.00  61.00  30.00   78
 29  ω    122.00 176.00   1.00   14.00    --  111.00  77.00  90.00   54
 30  ω     81.00 116.00   1.00   14.00    --  111.00  77.00  90.00   35
 31  ω    133.00 171.00   1.00   14.00    --  111.00  77.00-180.00   38
 32  ω     81.00 130.00   1.00   14.00    --  111.00  77.00-180.00   49
 33  ω     82.00 109.00   1.00   14.00    --  111.00  74.00 177.01   27
 34  ω     96.00 136.00   1.00   14.00    --  111.00 -61.00-150.00   40
 35  ω     85.00 111.00   1.00   14.00    --  111.00  61.00-120.00   26
 36  ω     44.00  92.00   1.00   14.00    --  111.00 -61.00-150.00   48
 37  ω     85.00 111.00   1.00   14.00    --  111.00  61.00 150.00   26
 38  ω     57.00 122.00   1.00   14.00    --  111.00-125.00  30.00   65
 39  ω     85.00 153.00   1.00   14.00    --  111.00  61.00-150.00   68
 40  ω     85.00 178.00   1.00   14.00    --  111.00  61.00 -90.00   93
 41  ω     81.00 107.00   1.00   14.00    --  111.00  77.00  30.00   26
 42  ω     81.00 107.00   1.00   14.00    --  111.00  77.00 -60.00   26
 43  ω     86.00 111.00   1.00   14.00    --  111.00  61.00  90.00   25
 44  ω     85.00 156.00   1.00   14.00    --  111.00  61.00 -60.00   71
 45  ω     81.00 170.00   1.00   14.00    --  111.00  77.00   0.00   89
 46  ω     81.00 177.00   1.00   14.00    --  111.00  77.00  60.00   96
 47  ω     81.00 107.00   1.00   14.00    --  111.00  77.00 150.00   26
 48  ω    142.00 168.00   1.00   14.00    --  111.00  77.00-120.00   26
 49  ω     90.00 118.00   1.00   14.00    --  111.00-121.00 157.00   28
 50  ω     63.00 109.00   1.00   14.00    --  111.00 -94.00 -90.00   46
 51  ω     32.00 106.00   1.00   14.00    --  111.00 -94.00  30.00   74
 52  ω     81.00 107.00   1.00   14.00    --  111.00  76.00-158.80   26
 53  ω     81.00 107.00   1.00   14.00    --  111.00  77.00 -90.00   26
 54  ω     84.00 176.00   1.00   14.00    --  111.00  63.00  39.99   92
 55  ω     83.00 110.00   1.00   14.00    --  111.00  67.00 -61.94   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0561159000
_diffrn_orient_matrix_UB_12      0.0701487000
_diffrn_orient_matrix_UB_13      0.0877659000
_diffrn_orient_matrix_UB_21      -0.0827323000
_diffrn_orient_matrix_UB_22      -0.0525470000
_diffrn_orient_matrix_UB_23      0.0296796000
_diffrn_orient_matrix_UB_31      0.0790652000
_diffrn_orient_matrix_UB_32      -0.0675387000
_diffrn_orient_matrix_UB_33      0.0098311000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10772
_reflns_number_total             12465
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.804
_refine_diff_density_min         -1.437
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12465
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0447
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0816P)²+1.6735P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1354
_refine_special_details          ?
_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
Br1 Br 0.23958(2) 0.31223(2) 0.11345(2) 0.02996(9) Uani 1 1 d . . . . .
Br2A Br 0.77327(8) 0.12432(5) 0.55514(4) 0.04368(17) Uani 0.6144(12) 1 d . . P
A 1
Br2B Br 0.72169(12) 0.11359(9) 0.53764(8) 0.04368(17) Uani 0.3856(12) 1 d . . P
A 2
N1 N 0.83572(13) 0.29287(12) -0.00460(10) 0.0162(3) Uani 1 1 d . . . . .
N2 N 0.79021(13) 0.23517(12) 0.08017(10) 0.0170(3) Uani 1 1 d . . . . .
C1 C 0.74884(15) 0.25264(13) 0.01326(11) 0.0157(4) Uani 1 1 d . . . . .
C2 C 0.93249(16) 0.30224(15) 0.05244(12) 0.0196(4) Uani 1 1 d . . . . .
H2 H 1.003644 0.328299 0.054029 0.024 Uiso 1 1 calc R . . . .
C4 C 0.83243(14) 0.32458(14) -0.07120(11) 0.0151(3) Uani 1 1 d . . . . .
C5 C 0.81074(15) 0.41549(14) -0.06213(11) 0.0166(4) Uani 1 1 d . . . . .
C3 C 0.90433(16) 0.26659(15) 0.10514(12) 0.0205(4) Uani 1 1 d . . . . .
H3 H 0.952444 0.263567 0.149969 0.025 Uiso 1 1 calc R . . . .
C6 C 0.81646(15) 0.44622(15) -0.12499(12) 0.0189(4) Uani 1 1 d . . . . .
H6 H 0.803025 0.506462 -0.121024 0.023 Uiso 1 1 calc R . . . .
C7 C 0.84190(16) 0.38825(15) -0.19331(12) 0.0200(4) Uani 1 1 d . . . . .
H7 H 0.847201 0.410631 -0.233977 0.024 Uiso 1 1 calc R . . . .
C8 C 0.85950(16) 0.29718(15) -0.20154(12) 0.0209(4) Uani 1 1 d . . . . .
H8 H 0.874550 0.258598 -0.248394 0.025 Uiso 1 1 calc R . . . .
C9 C 0.85500(15) 0.26250(14) -0.14078(12) 0.0180(4) Uani 1 1 d . . . . .
C10 C 0.78126(15) 0.48010(14) 0.01158(11) 0.0179(4) Uani 1 1 d . . . . .
H10 H 0.781396 0.447251 0.049237 0.021 Uiso 1 1 calc R . . . .
C11 C 0.86745(17) 0.57484(15) 0.05439(13) 0.0231(4) Uani 1 1 d . . . . .
H11A H 0.939693 0.561406 0.068249 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.850574 0.613179 0.102700 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.865962 0.609181 0.019005 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.66543(17) 0.49962(16) -0.01301(13) 0.0223(4) Uani 1 1 d . . . . .
H12A H 0.664384 0.532806 -0.049234 0.033 Uiso 1 1 calc GR . . . .
H12B H 0.646869 0.538484 0.034329 0.033 Uiso 1 1 calc GR . . . .
H12C H 0.612482 0.439804 -0.039542 0.033 Uiso 1 1 calc GR . . . .
C13 C 0.87397(17) 0.16231(15) -0.15066(13) 0.0216(4) Uani 1 1 d . . . . .
H13 H 0.848705 0.145351 -0.109325 0.026 Uiso 1 1 calc R . . . .
C14 C 0.8075(2) 0.08656(17) -0.23391(14) 0.0310(5) Uani 1 1 d . . . . .
H14A H 0.730675 0.089429 -0.242352 0.046 Uiso 1 1 calc GR . . . .
H14B H 0.816308 0.023812 -0.235949 0.046 Uiso 1 1 calc GR . . . .
H14C H 0.834137 0.099168 -0.275388 0.046 Uiso 1 1 calc GR . . . .
C15 C 0.99743(19) 0.16053(17) -0.13677(15) 0.0297(5) Uani 1 1 d . . . . .
H15A H 1.025069 0.179899 -0.174998 0.045 Uiso 1 1 calc GR . . . .
H15B H 1.007500 0.096661 -0.143753 0.045 Uiso 1 1 calc GR . . . .
H15C H 1.037025 0.203929 -0.082840 0.045 Uiso 1 1 calc GR . . . .
C16 C 0.73332(16) 0.17198(14) 0.11026(12) 0.0193(4) Uani 1 1 d . . . . .
C17 C 0.71910(18) 0.07276(15) 0.06777(13) 0.0243(4) Uani 1 1 d . . . . .
C18 C 0.6710(2) 0.01219(16) 0.10021(15) 0.0304(5) Uani 1 1 d . . . . .
H18 H 0.658638 -0.054014 0.073192 0.036 Uiso 1 1 calc R . . . .
C19 C 0.6416(2) 0.04871(17) 0.17111(15) 0.0321(5) Uani 1 1 d . . . . .
H19 H 0.611484 0.007165 0.192147 0.039 Uiso 1 1 calc R . . . .
C20 C 0.6568(2) 0.14723(17) 0.21150(14) 0.0293(5) Uani 1 1 d . . . . .
H20 H 0.635871 0.170900 0.259129 0.035 Uiso 1 1 calc R . . . .
C21 C 0.70291(18) 0.21156(15) 0.18178(13) 0.0232(4) Uani 1 1 d . . . . .
C22 C 0.7541(2) 0.03026(17) -0.00870(15) 0.0345(5) Uani 1 1 d . . . . .
H22 H 0.790878 0.083412 -0.019187 0.041 Uiso 1 1 calc R . . . .
C23 C 0.6569(3) -0.0255(3) -0.08036(18) 0.0639(10) Uani 1 1 d . . . . .
H23A H 0.625093 -0.082665 -0.074776 0.096 Uiso 1 1 calc GR . . . .
H23B H 0.680842 -0.042700 -0.128824 0.096 Uiso 1 1 calc GR . . . .
H23C H 0.602559 0.013232 -0.083369 0.096 Uiso 1 1 calc GR . . . .
C24 C 0.8383(3) -0.0345(2) 0.00115(19) 0.0494(7) Uani 1 1 d . . . . .
H24A H 0.899636 0.001427 0.047651 0.074 Uiso 1 1 calc GR . . . .
H24B H 0.864458 -0.055420 -0.046246 0.074 Uiso 1 1 calc GR . . . .
H24C H 0.802795 -0.089366 0.008122 0.074 Uiso 1 1 calc GR . . . .
C25 C 0.71948(19) 0.31897(16) 0.22791(13) 0.0263(4) Uani 1 1 d . . . . .
H25 H 0.735117 0.351472 0.192340 0.032 Uiso 1 1 calc R . . . .
C26 C 0.8191(2) 0.35392(18) 0.30285(14) 0.0346(5) Uani 1 1 d . . . . .
H26A H 0.806756 0.321244 0.337745 0.052 Uiso 1 1 calc GR . . . .
H26B H 0.828446 0.421844 0.331281 0.052 Uiso 1 1 calc GR . . . .
H26C H 0.884585 0.340530 0.286425 0.052 Uiso 1 1 calc GR . . . .
C27 C 0.6152(2) 0.34660(18) 0.25251(15) 0.0332(5) Uani 1 1 d . . . . .
H27A H 0.553031 0.322818 0.205360 0.050 Uiso 1 1 calc GR . . . .
H27B H 0.626472 0.415250 0.277205 0.050 Uiso 1 1 calc GR . . . .
H27C H 0.601090 0.318953 0.290277 0.050 Uiso 1 1 calc GR . . . .
C28 C 0.63176(15) 0.23838(14) -0.02770(12) 0.0176(4) Uani 1 1 d . . . . .
C29 C 0.55760(17) 0.26439(15) 0.01870(13) 0.0211(4) Uani 1 1 d . . . . .
H29 H 0.582277 0.286931 0.074800 0.025 Uiso 1 1 calc R . . . .
C30 C 0.44699(17) 0.25667(16) -0.01876(15) 0.0258(4) Uani 1 1 d . . . . .
H30 H 0.398223 0.274304 0.012506 0.031 Uiso 1 1 calc R . . . .
C31 C 0.40890(17) 0.22279(15) -0.10254(15) 0.0258(4) Uani 1 1 d . . . . .
C32 C 0.48309(18) 0.19640(16) -0.14829(13) 0.0255(4) Uani 1 1 d . . . . .
H32 H 0.458019 0.173269 -0.204397 0.031 Uiso 1 1 calc R . . . .
C33 C 0.59355(16) 0.20386(15) -0.11198(12) 0.0211(4) Uani 1 1 d . . . . .
H33 H 0.641962 0.186009 -0.143516 0.025 Uiso 1 1 calc R . . . .
C34 C 0.28910(19) 0.2145(2) -0.14318(19) 0.0390(6) Uani 1 1 d . . . . .
H34A H 0.283897 0.257875 -0.170927 0.059 Uiso 1 1 calc GR . . . .
H34B H 0.248849 0.230473 -0.103171 0.059 Uiso 1 1 calc GR . . . .
H34C H 0.258300 0.149888 -0.181319 0.059 Uiso 1 1 calc GR . . . .
N3 N 0.71686(13) 0.73093(12) 0.41610(10) 0.0188(3) Uani 1 1 d . . . . .
N4 N 0.78874(14) 0.80562(12) 0.54508(10) 0.0189(3) Uani 1 1 d . . . . .
C35 C 0.76241(15) 0.71837(14) 0.48424(11) 0.0176(4) Uani 1 1 d . . . . .
C36 C 0.71381(17) 0.82675(16) 0.43376(13) 0.0234(4) Uani 1 1 d . . . . .
H36 H 0.686403 0.853878 0.397092 0.028 Uiso 1 1 calc R . . . .
C37 C 0.75832(17) 0.87366(15) 0.51462(13) 0.0232(4) Uani 1 1 d . . . . .
H37 H 0.766830 0.938965 0.544021 0.028 Uiso 1 1 calc R . . . .
C38 C 0.67505(16) 0.65704(14) 0.33485(11) 0.0184(4) Uani 1 1 d . . . . .
C39 C 0.56068(17) 0.62783(15) 0.30276(12) 0.0219(4) Uani 1 1 d . . . . .
C40 C 0.52057(18) 0.56113(17) 0.22306(13) 0.0271(4) Uani 1 1 d . . . . .
H40 H 0.444687 0.539836 0.199722 0.033 Uiso 1 1 calc R . . . .
C41 C 0.5930(2) 0.52663(16) 0.17869(13) 0.0280(5) Uani 1 1 d . . . . .
H41 H 0.565327 0.483115 0.125430 0.034 Uiso 1 1 calc R . . . .
C42 C 0.70652(19) 0.55622(16) 0.21280(13) 0.0253(4) Uani 1 1 d . . . . .
H42 H 0.753796 0.531563 0.182131 0.030 Uiso 1 1 calc R . . . .
C43 C 0.75109(17) 0.62221(15) 0.29215(12) 0.0207(4) Uani 1 1 d . . . . .
C44 C 0.47959(18) 0.66683(18) 0.34942(14) 0.0280(5) Uani 1 1 d . . . . .
H44 H 0.521111 0.703157 0.406080 0.034 Uiso 1 1 calc R . . . .
C45 C 0.4261(2) 0.7364(2) 0.31633(17) 0.0360(5) Uani 1 1 d . . . . .
H45A H 0.482417 0.789097 0.323184 0.054 Uiso 1 1 calc GR . . . .
H45B H 0.373942 0.760280 0.345268 0.054 Uiso 1 1 calc GR . . . .
H45C H 0.388594 0.703097 0.259900 0.054 Uiso 1 1 calc GR . . . .
C46 C 0.3920(2) 0.5862(2) 0.34645(17) 0.0377(6) Uani 1 1 d . . . . .
H46A H 0.352008 0.548175 0.291207 0.057 Uiso 1 1 calc GR . . . .
H46B H 0.341638 0.613399 0.375825 0.057 Uiso 1 1 calc GR . . . .
H46C H 0.427361 0.546309 0.370453 0.057 Uiso 1 1 calc GR . . . .
C47 C 0.87552(18) 0.65762(18) 0.32886(13) 0.0274(5) Uani 1 1 d . . . . .
H47 H 0.892253 0.664302 0.385530 0.033 Uiso 1 1 calc R . . . .
C48 C 0.9423(2) 0.5884(2) 0.28694(18) 0.0395(6) Uani 1 1 d . . . . .
H48A H 0.917209 0.525744 0.286151 0.059 Uiso 1 1 calc GR . . . .
H48B H 1.019267 0.611020 0.315858 0.059 Uiso 1 1 calc GR . . . .
H48C H 0.932384 0.584943 0.232496 0.059 Uiso 1 1 calc GR . . . .
C49 C 0.9138(2) 0.7559(2) 0.32733(19) 0.0416(6) Uani 1 1 d . . . . .
H49A H 0.904781 0.750076 0.272354 0.062 Uiso 1 1 calc GR . . . .
H49B H 0.990432 0.780135 0.356904 0.062 Uiso 1 1 calc GR . . . .
H49C H 0.870485 0.799269 0.351751 0.062 Uiso 1 1 calc GR . . . .
C50 C 0.83834(17) 0.82577(14) 0.62973(12) 0.0195(4) Uani 1 1 d . . . . .
C51 C 0.95102(17) 0.86942(15) 0.66151(13) 0.0226(4) Uani 1 1 d . . . . .
C52 C 0.99747(19) 0.88871(16) 0.74340(13) 0.0274(5) Uani 1 1 d . . . . .
H52 H 1.071871 0.917781 0.767278 0.033 Uiso 1 1 calc R . . . .
C53 C 0.9335(2) 0.86484(16) 0.78921(13) 0.0283(5) Uani 1 1 d . . . . .
H53 H 0.965720 0.878284 0.843547 0.034 Uiso 1 1 calc R . . . .
C54 C 0.8229(2) 0.82156(15) 0.75580(13) 0.0262(4) Uani 1 1 d . . . . .
H54 H 0.781835 0.805610 0.787623 0.031 Uiso 1 1 calc R . . . .
C55 C 0.77213(18) 0.80154(15) 0.67473(12) 0.0228(4) Uani 1 1 d . . . . .
C56 C 1.02092(18) 0.89233(17) 0.60987(14) 0.0283(5) Uani 1 1 d . . . . .
H56 H 0.980571 0.855424 0.553045 0.034 Uiso 1 1 calc R . . . .
C57 C 1.1324(2) 0.8622(2) 0.62527(19) 0.0400(6) Uani 1 1 d . . . . .
H57A H 1.177895 0.903569 0.678222 0.060 Uiso 1 1 calc GR . . . .
H57B H 1.168669 0.867211 0.585457 0.060 Uiso 1 1 calc GR . . . .
H57C H 1.120420 0.797041 0.621776 0.060 Uiso 1 1 calc GR . . . .
C58 C 1.0389(2) 0.99840(19) 0.62296(18) 0.0386(6) Uani 1 1 d . . . . .
H58A H 0.968652 1.016599 0.613530 0.058 Uiso 1 1 calc GR . . . .
H58B H 1.077536 1.009300 0.586080 0.058 Uiso 1 1 calc GR . . . .
H58C H 1.081974 1.036139 0.677524 0.058 Uiso 1 1 calc GR . . . .
C59 C 0.64982(19) 0.75427(16) 0.63901(14) 0.0271(5) Uani 1 1 d . . . . .
H59 H 0.630179 0.742487 0.581213 0.033 Uiso 1 1 calc R . . . .
C60 C 0.5780(2) 0.8203(2) 0.6785(2) 0.0447(7) Uani 1 1 d . . . . .
H60A H 0.596750 0.833567 0.735469 0.067 Uiso 1 1 calc GR . . . .
H60B H 0.501408 0.789349 0.654595 0.067 Uiso 1 1 calc GR . . . .
H60C H 0.590957 0.879416 0.670353 0.067 Uiso 1 1 calc GR . . . .
C61 C 0.6275(2) 0.65716(18) 0.64770(15) 0.0334(5) Uani 1 1 d . . . . .
H61A H 0.674343 0.617516 0.623531 0.050 Uiso 1 1 calc GR . . . .
H61B H 0.551414 0.625901 0.621020 0.050 Uiso 1 1 calc GR . . . .
H61C H 0.642762 0.667359 0.703992 0.050 Uiso 1 1 calc GR . . . .
C62 C 0.77859(16) 0.62804(14) 0.49302(11) 0.0182(4) Uani 1 1 d . . . . .
C63 C 0.88026(17) 0.62150(15) 0.53685(12) 0.0220(4) Uani 1 1 d . . . . .
H63 H 0.939129 0.674187 0.559196 0.026 Uiso 1 1 calc R . . . .
C64 C 0.89369(18) 0.53707(16) 0.54713(13) 0.0242(4) Uani 1 1 d . . . . .
H64 H 0.962021 0.533433 0.575958 0.029 Uiso 1 1 calc R . . . .
C65 C 0.80617(19) 0.45675(16) 0.51489(13) 0.0244(4) Uani 1 1 d . . . . .
C66 C 0.70549(18) 0.46468(15) 0.47192(13) 0.0239(4) Uani 1 1 d . . . . .
H66 H 0.646358 0.412254 0.450343 0.029 Uiso 1 1 calc R . . . .
C67 C 0.69052(17) 0.54831(15) 0.46023(12) 0.0224(4) Uani 1 1 d . . . . .
H67 H 0.622395 0.551507 0.430784 0.027 Uiso 1 1 calc R . . . .
C68 C 0.8215(2) 0.36515(18) 0.52631(16) 0.0333(5) Uani 1 1 d . . . . .
H68A H 0.891153 0.351575 0.517857 0.050 Uiso 1 1 calc GR . . . .
H68B H 0.762655 0.313345 0.488120 0.050 Uiso 1 1 calc GR . . . .
H68C H 0.820596 0.372007 0.580265 0.050 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
N1 C1 1.350(2) . ?
N1 C2 1.385(3) . ?
N1 C4 1.452(2) . ?
N2 C1 1.352(3) . ?
N2 C3 1.388(3) . ?
N2 C16 1.454(2) . ?
C1 C28 1.463(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.347(3) . ?
C4 C5 1.398(3) . ?
C4 C9 1.408(3) . ?
C5 C6 1.395(3) . ?
C5 C10 1.520(3) . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.387(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.387(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.394(3) . ?
C9 C13 1.521(3) . ?
C10 H10 0.9800 . ?
C10 C11 1.535(3) . ?
C10 C12 1.533(3) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.538(3) . ?
C13 C15 1.533(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.404(3) . ?
C16 C21 1.397(3) . ?
C17 C18 1.403(3) . ?
C17 C22 1.511(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.375(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.388(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.399(3) . ?
C21 C25 1.519(3) . ?
C22 H22 0.9800 . ?
C22 C23 1.499(4) . ?
C22 C24 1.555(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.534(3) . ?
C25 C27 1.541(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.399(3) . ?
C28 C33 1.398(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.392(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.390(3) . ?
C31 C32 1.392(3) . ?
C31 C34 1.508(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.386(3) . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
N3 C35 1.344(3) . ?
N3 C36 1.383(3) . ?
N3 C38 1.457(2) . ?
N4 C35 1.350(3) . ?
N4 C37 1.386(3) . ?
N4 C50 1.450(3) . ?
C35 C62 1.466(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.356(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.393(3) . ?
C38 C43 1.405(3) . ?
C39 C40 1.398(3) . ?
C39 C44 1.517(3) . ?
C40 H40 0.9300 . ?
C40 C41 1.383(3) . ?
C41 H41 0.9300 . ?
C41 C42 1.388(3) . ?
C42 H42 0.9300 . ?
C42 C43 1.395(3) . ?
C43 C47 1.522(3) . ?
C44 H44 0.9800 . ?
C44 C45 1.540(4) . ?
C44 C46 1.529(3) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47 0.9800 . ?
C47 C48 1.528(3) . ?
C47 C49 1.524(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.402(3) . ?
C50 C55 1.396(3) . ?
C51 C52 1.400(3) . ?
C51 C56 1.520(3) . ?
C52 H52 0.9300 . ?
C52 C53 1.387(3) . ?
C53 H53 0.9300 . ?
C53 C54 1.380(3) . ?
C54 H54 0.9300 . ?
C54 C55 1.394(3) . ?
C55 C59 1.523(3) . ?
C56 H56 0.9800 . ?
C56 C57 1.532(3) . ?
C56 C58 1.524(3) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 H59 0.9800 . ?
C59 C60 1.533(3) . ?
C59 C61 1.535(3) . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 C63 1.397(3) . ?
C62 C67 1.400(3) . ?
C63 H63 0.9300 . ?
C63 C64 1.381(3) . ?
C64 H64 0.9300 . ?
C64 C65 1.402(3) . ?
C65 C66 1.389(3) . ?
C65 C68 1.503(3) . ?
C66 H66 0.9300 . ?
C66 C67 1.385(3) . ?
C67 H67 0.9300 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 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
C1 N1 C2 109.40(16) . . ?
C1 N1 C4 127.12(16) . . ?
C2 N1 C4 123.47(16) . . ?
C1 N2 C3 109.15(16) . . ?
C1 N2 C16 126.60(16) . . ?
C3 N2 C16 122.39(17) . . ?
N1 C1 N2 106.89(16) . . ?
N1 C1 C28 126.50(17) . . ?
N2 C1 C28 126.41(17) . . ?
N1 C2 H2 126.4 . . ?
C3 C2 N1 107.24(17) . . ?
C3 C2 H2 126.4 . . ?
C5 C4 N1 118.75(16) . . ?
C5 C4 C9 123.62(17) . . ?
C9 C4 N1 117.60(17) . . ?
C4 C5 C10 123.22(17) . . ?
C6 C5 C4 117.00(17) . . ?
C6 C5 C10 119.78(18) . . ?
N2 C3 H3 126.3 . . ?
C2 C3 N2 107.31(17) . . ?
C2 C3 H3 126.3 . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 120.95(19) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.59(18) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.11(18) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C13 122.71(18) . . ?
C8 C9 C4 116.68(18) . . ?
C8 C9 C13 120.61(18) . . ?
C5 C10 H10 108.5 . . ?
C5 C10 C11 110.31(16) . . ?
C5 C10 C12 110.42(16) . . ?
C11 C10 H10 108.5 . . ?
C12 C10 H10 108.5 . . ?
C12 C10 C11 110.44(17) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 107.8 . . ?
C9 C13 C14 112.02(18) . . ?
C9 C13 C15 110.82(16) . . ?
C14 C13 H13 107.8 . . ?
C15 C13 H13 107.8 . . ?
C15 C13 C14 110.33(18) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 116.97(18) . . ?
C21 C16 N2 119.42(18) . . ?
C21 C16 C17 123.45(19) . . ?
C16 C17 C22 123.30(19) . . ?
C18 C17 C16 116.7(2) . . ?
C18 C17 C22 120.0(2) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.3(2) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 119.8 . . ?
C18 C19 C20 120.4(2) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.1(2) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C20 116.9(2) . . ?
C16 C21 C25 123.22(18) . . ?
C20 C21 C25 119.82(19) . . ?
C17 C22 H22 107.8 . . ?
C17 C22 C24 111.3(2) . . ?
C23 C22 C17 111.9(2) . . ?
C23 C22 H22 107.8 . . ?
C23 C22 C24 110.0(2) . . ?
C24 C22 H22 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 108.0 . . ?
C21 C25 C26 110.5(2) . . ?
C21 C25 C27 111.88(18) . . ?
C26 C25 H25 108.0 . . ?
C26 C25 C27 110.24(19) . . ?
C27 C25 H25 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 119.14(18) . . ?
C33 C28 C1 121.41(18) . . ?
C33 C28 C29 119.37(18) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.2(2) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.8 . . ?
C31 C30 C29 120.5(2) . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C32 118.89(19) . . ?
C30 C31 C34 120.5(2) . . ?
C32 C31 C34 120.6(2) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.4(2) . . ?
C33 C32 H32 119.3 . . ?
C28 C33 H33 120.2 . . ?
C32 C33 C28 119.62(19) . . ?
C32 C33 H33 120.2 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 N3 C36 109.76(17) . . ?
C35 N3 C38 126.84(17) . . ?
C36 N3 C38 123.39(17) . . ?
C35 N4 C37 109.50(17) . . ?
C35 N4 C50 125.81(17) . . ?
C37 N4 C50 124.67(17) . . ?
N3 C35 N4 106.81(17) . . ?
N3 C35 C62 127.61(18) . . ?
N4 C35 C62 125.57(18) . . ?
N3 C36 H36 126.5 . . ?
C37 C36 N3 107.06(19) . . ?
C37 C36 H36 126.5 . . ?
N4 C37 H37 126.6 . . ?
C36 C37 N4 106.87(18) . . ?
C36 C37 H37 126.6 . . ?
C39 C38 N3 117.45(17) . . ?
C39 C38 C43 123.73(18) . . ?
C43 C38 N3 118.77(17) . . ?
C38 C39 C40 117.43(19) . . ?
C38 C39 C44 123.09(19) . . ?
C40 C39 C44 119.46(19) . . ?
C39 C40 H40 119.8 . . ?
C41 C40 C39 120.4(2) . . ?
C41 C40 H40 119.8 . . ?
C40 C41 H41 119.6 . . ?
C40 C41 C42 120.7(2) . . ?
C42 C41 H41 119.6 . . ?
C41 C42 H42 119.4 . . ?
C41 C42 C43 121.3(2) . . ?
C43 C42 H42 119.4 . . ?
C38 C43 C47 122.06(19) . . ?
C42 C43 C38 116.40(19) . . ?
C42 C43 C47 121.49(19) . . ?
C39 C44 H44 108.1 . . ?
C39 C44 C45 109.45(19) . . ?
C39 C44 C46 111.7(2) . . ?
C45 C44 H44 108.1 . . ?
C46 C44 H44 108.1 . . ?
C46 C44 C45 111.3(2) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C47 H47 107.8 . . ?
C43 C47 C48 113.1(2) . . ?
C43 C47 C49 111.2(2) . . ?
C48 C47 H47 107.8 . . ?
C49 C47 H47 107.8 . . ?
C49 C47 C48 108.8(2) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 N4 117.28(18) . . ?
C55 C50 N4 118.76(18) . . ?
C55 C50 C51 123.95(19) . . ?
C50 C51 C56 122.29(19) . . ?
C52 C51 C50 116.5(2) . . ?
C52 C51 C56 121.15(19) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 C51 120.5(2) . . ?
C53 C52 H52 119.7 . . ?
C52 C53 H53 119.3 . . ?
C54 C53 C52 121.3(2) . . ?
C54 C53 H53 119.3 . . ?
C53 C54 H54 119.7 . . ?
C53 C54 C55 120.5(2) . . ?
C55 C54 H54 119.7 . . ?
C50 C55 C59 123.09(19) . . ?
C54 C55 C50 117.1(2) . . ?
C54 C55 C59 119.8(2) . . ?
C51 C56 H56 107.7 . . ?
C51 C56 C57 111.7(2) . . ?
C51 C56 C58 111.6(2) . . ?
C57 C56 H56 107.7 . . ?
C58 C56 H56 107.7 . . ?
C58 C56 C57 110.2(2) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C55 C59 H59 108.1 . . ?
C55 C59 C60 111.03(19) . . ?
C55 C59 C61 110.5(2) . . ?
C60 C59 H59 108.1 . . ?
C60 C59 C61 110.9(2) . . ?
C61 C59 H59 108.1 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C35 120.62(18) . . ?
C63 C62 C67 119.2(2) . . ?
C67 C62 C35 120.13(18) . . ?
C62 C63 H63 119.9 . . ?
C64 C63 C62 120.25(19) . . ?
C64 C63 H63 119.9 . . ?
C63 C64 H64 119.4 . . ?
C63 C64 C65 121.2(2) . . ?
C65 C64 H64 119.4 . . ?
C64 C65 C68 120.8(2) . . ?
C66 C65 C64 117.8(2) . . ?
C66 C65 C68 121.4(2) . . ?
C65 C66 H66 119.0 . . ?
C67 C66 C65 121.9(2) . . ?
C67 C66 H66 119.0 . . ?
C62 C67 H67 120.2 . . ?
C66 C67 C62 119.6(2) . . ?
C66 C67 H67 120.2 . . ?
C65 C68 H68A 109.5 . . ?
C65 C68 H68B 109.5 . . ?
C65 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C28 C29 -133.1(2) . . . . ?
N1 C1 C28 C33 43.7(3) . . . . ?
N1 C2 C3 N2 0.1(2) . . . . ?
N1 C4 C5 C6 175.33(16) . . . . ?
N1 C4 C5 C10 -5.0(3) . . . . ?
N1 C4 C9 C8 -175.39(16) . . . . ?
N1 C4 C9 C13 4.5(3) . . . . ?
N2 C1 C28 C29 41.1(3) . . . . ?
N2 C1 C28 C33 -142.1(2) . . . . ?
N2 C16 C17 C18 175.77(19) . . . . ?
N2 C16 C17 C22 -3.4(3) . . . . ?
N2 C16 C21 C20 -174.81(19) . . . . ?
N2 C16 C21 C25 4.1(3) . . . . ?
C1 N1 C2 C3 0.5(2) . . . . ?
C1 N1 C4 C5 83.1(2) . . . . ?
C1 N1 C4 C9 -98.9(2) . . . . ?
C1 N2 C3 C2 -0.8(2) . . . . ?
C1 N2 C16 C17 73.9(3) . . . . ?
C1 N2 C16 C21 -110.5(2) . . . . ?
C1 C28 C29 C30 176.33(18) . . . . ?
C1 C28 C33 C32 -176.43(19) . . . . ?
C2 N1 C1 N2 -1.0(2) . . . . ?
C2 N1 C1 C28 174.18(18) . . . . ?
C2 N1 C4 C5 -95.4(2) . . . . ?
C2 N1 C4 C9 82.6(2) . . . . ?
C4 N1 C1 N2 -179.67(17) . . . . ?
C4 N1 C1 C28 -4.5(3) . . . . ?
C4 N1 C2 C3 179.27(18) . . . . ?
C4 C5 C6 C7 0.4(3) . . . . ?
C4 C5 C10 C11 119.4(2) . . . . ?
C4 C5 C10 C12 -118.3(2) . . . . ?
C4 C9 C13 C14 133.1(2) . . . . ?
C4 C9 C13 C15 -103.2(2) . . . . ?
C5 C4 C9 C8 2.5(3) . . . . ?
C5 C4 C9 C13 -177.56(17) . . . . ?
C5 C6 C7 C8 1.6(3) . . . . ?
C3 N2 C1 N1 1.1(2) . . . . ?
C3 N2 C1 C28 -174.10(18) . . . . ?
C3 N2 C16 C17 -88.8(2) . . . . ?
C3 N2 C16 C21 86.7(3) . . . . ?
C6 C5 C10 C11 -61.0(2) . . . . ?
C6 C5 C10 C12 61.3(2) . . . . ?
C6 C7 C8 C9 -1.7(3) . . . . ?
C7 C8 C9 C4 -0.3(3) . . . . ?
C7 C8 C9 C13 179.74(18) . . . . ?
C8 C9 C13 C14 -47.0(3) . . . . ?
C8 C9 C13 C15 76.7(2) . . . . ?
C9 C4 C5 C6 -2.5(3) . . . . ?
C9 C4 C5 C10 177.09(17) . . . . ?
C10 C5 C6 C7 -179.24(17) . . . . ?
C16 N2 C1 N1 -163.57(18) . . . . ?
C16 N2 C1 C28 21.3(3) . . . . ?
C16 N2 C3 C2 164.66(18) . . . . ?
C16 C17 C18 C19 -1.4(4) . . . . ?
C16 C17 C22 C23 -114.8(3) . . . . ?
C16 C17 C22 C24 121.7(3) . . . . ?
C16 C21 C25 C26 -103.4(2) . . . . ?
C16 C21 C25 C27 133.3(2) . . . . ?
C17 C16 C21 C20 0.5(3) . . . . ?
C17 C16 C21 C25 179.4(2) . . . . ?
C17 C18 C19 C20 1.6(4) . . . . ?
C18 C17 C22 C23 66.0(3) . . . . ?
C18 C17 C22 C24 -57.5(3) . . . . ?
C18 C19 C20 C21 -0.6(4) . . . . ?
C19 C20 C21 C16 -0.4(4) . . . . ?
C19 C20 C21 C25 -179.3(2) . . . . ?
C20 C21 C25 C26 75.5(3) . . . . ?
C20 C21 C25 C27 -47.7(3) . . . . ?
C21 C16 C17 C18 0.4(3) . . . . ?
C21 C16 C17 C22 -178.8(2) . . . . ?
C22 C17 C18 C19 177.8(2) . . . . ?
C28 C29 C30 C31 0.2(3) . . . . ?
C29 C28 C33 C32 0.3(3) . . . . ?
C29 C30 C31 C32 0.3(3) . . . . ?
C29 C30 C31 C34 -179.9(2) . . . . ?
C30 C31 C32 C33 -0.4(3) . . . . ?
C31 C32 C33 C28 0.1(3) . . . . ?
C33 C28 C29 C30 -0.5(3) . . . . ?
C34 C31 C32 C33 179.8(2) . . . . ?
N3 C35 C62 C63 132.6(2) . . . . ?
N3 C35 C62 C67 -50.1(3) . . . . ?
N3 C36 C37 N4 0.4(2) . . . . ?
N3 C38 C39 C40 176.29(19) . . . . ?
N3 C38 C39 C44 -2.1(3) . . . . ?
N3 C38 C43 C42 -175.94(18) . . . . ?
N3 C38 C43 C47 1.4(3) . . . . ?
N4 C35 C62 C63 -49.3(3) . . . . ?
N4 C35 C62 C67 128.1(2) . . . . ?
N4 C50 C51 C52 179.75(18) . . . . ?
N4 C50 C51 C56 -2.0(3) . . . . ?
N4 C50 C55 C54 179.68(18) . . . . ?
N4 C50 C55 C59 0.3(3) . . . . ?
C35 N3 C36 C37 -0.1(2) . . . . ?
C35 N3 C38 C39 105.5(2) . . . . ?
C35 N3 C38 C43 -77.0(3) . . . . ?
C35 N4 C37 C36 -0.6(2) . . . . ?
C35 N4 C50 C51 104.5(2) . . . . ?
C35 N4 C50 C55 -75.9(3) . . . . ?
C35 C62 C63 C64 177.81(19) . . . . ?
C35 C62 C67 C66 -177.21(18) . . . . ?
C36 N3 C35 N4 -0.2(2) . . . . ?
C36 N3 C35 C62 178.20(19) . . . . ?
C36 N3 C38 C39 -73.9(3) . . . . ?
C36 N3 C38 C43 103.5(2) . . . . ?
C37 N4 C35 N3 0.5(2) . . . . ?
C37 N4 C35 C62 -177.96(18) . . . . ?
C37 N4 C50 C51 -77.3(3) . . . . ?
C37 N4 C50 C55 102.3(2) . . . . ?
C38 N3 C35 N4 -179.74(17) . . . . ?
C38 N3 C35 C62 -1.3(3) . . . . ?
C38 N3 C36 C37 179.39(18) . . . . ?
C38 C39 C40 C41 -0.2(3) . . . . ?
C38 C39 C44 C45 106.1(2) . . . . ?
C38 C39 C44 C46 -130.1(2) . . . . ?
C38 C43 C47 C48 159.6(2) . . . . ?
C38 C43 C47 C49 -77.6(3) . . . . ?
C39 C38 C43 C42 1.3(3) . . . . ?
C39 C38 C43 C47 178.7(2) . . . . ?
C39 C40 C41 C42 1.1(4) . . . . ?
C40 C39 C44 C45 -72.3(3) . . . . ?
C40 C39 C44 C46 51.5(3) . . . . ?
C40 C41 C42 C43 -0.8(4) . . . . ?
C41 C42 C43 C38 -0.4(3) . . . . ?
C41 C42 C43 C47 -177.8(2) . . . . ?
C42 C43 C47 C48 -23.2(3) . . . . ?
C42 C43 C47 C49 99.6(3) . . . . ?
C43 C38 C39 C40 -1.0(3) . . . . ?
C43 C38 C39 C44 -179.4(2) . . . . ?
C44 C39 C40 C41 178.2(2) . . . . ?
C50 N4 C35 N3 178.95(17) . . . . ?
C50 N4 C35 C62 0.5(3) . . . . ?
C50 N4 C37 C36 -179.06(18) . . . . ?
C50 C51 C52 C53 0.2(3) . . . . ?
C50 C51 C56 C57 -134.4(2) . . . . ?
C50 C51 C56 C58 101.8(2) . . . . ?
C50 C55 C59 C60 -115.8(2) . . . . ?
C50 C55 C59 C61 120.7(2) . . . . ?
C51 C50 C55 C54 -0.7(3) . . . . ?
C51 C50 C55 C59 179.9(2) . . . . ?
C51 C52 C53 C54 0.1(3) . . . . ?
C52 C51 C56 C57 43.8(3) . . . . ?
C52 C51 C56 C58 -80.1(3) . . . . ?
C52 C53 C54 C55 -0.7(3) . . . . ?
C53 C54 C55 C50 1.0(3) . . . . ?
C53 C54 C55 C59 -179.6(2) . . . . ?
C54 C55 C59 C60 64.9(3) . . . . ?
C54 C55 C59 C61 -58.6(3) . . . . ?
C55 C50 C51 C52 0.1(3) . . . . ?
C55 C50 C51 C56 178.4(2) . . . . ?
C56 C51 C52 C53 -178.1(2) . . . . ?
C62 C63 C64 C65 -0.7(3) . . . . ?
C63 C62 C67 C66 0.2(3) . . . . ?
C63 C64 C65 C66 0.3(3) . . . . ?
C63 C64 C65 C68 180.0(2) . . . . ?
C64 C65 C66 C67 0.4(3) . . . . ?
C65 C66 C67 C62 -0.6(3) . . . . ?
C67 C62 C63 C64 0.4(3) . . . . ?
C68 C65 C66 C67 -179.3(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.116 0.416 0.267 34.1 8.8 ?
2 -0.116 0.584 0.733 34.1 8.7 ?
3 0.500 0.000 0.500 178.2 47.5 ?

_olex2_date_sample_data_collection 2017-01-22
_olex2_date_sample_submission    1484780400
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Br2A) = Uanis(Br2B)
3. Others
 Sof(Br2B)=1-FVAR(1)
 Sof(Br2A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C44(H44), C47(H47), C56(H56), C59(H59)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30), C32(H32), C33(H33), C36(H36), C37(H37), C40(H40), C41(H41),
  C42(H42), C52(H52), C53(H53), C54(H54), C63(H63), C64(H64), C66(H66), C67(H67)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C68(H68A,H68B,H68C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.178
_oxdiff_exptl_absorpt_empirical_full_min 0.891
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
####################################################################### 
# 
# 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_compound_3a
_database_code_depnum_ccdc_archive 'CCDC 1559107'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;

_audit_creation_date             2017-01-23
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H41 N2, Br'
_chemical_formula_sum            'C33 H41 Br N2'
_chemical_formula_weight         545.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H41 Br N2'
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'
Br Br -0.6763 1.2805 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   30.08483(19)
_cell_length_b                   8.95600(6)
_cell_length_c                   22.48986(13)
_cell_angle_alpha                90
_cell_angle_beta                 95.3846(6)
_cell_angle_gamma                90
_cell_volume                     6032.92(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    39104
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      72.2560
_cell_measurement_theta_min      2.8990
_exptl_absorpt_coefficient_mu    2.008
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2304.0
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 4 -2 0.1214
-1 1 0 0.1414
0 0 -1 0.1468
0 0 1 0.1468
-2 5 4 0.1753
1 -1 0 0.1414
1 0 0 0.1080
-1 0 0 0.1080
-5 -3 -3 0.1582

_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.216
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.9943 3.9960 -2.0115 0.4468 0.4015 -0.4509
-0.9990 0.9992 -0.0032 0.1046 0.0671 -0.1293
0.0004 -0.0005 -0.9993 -0.0094 0.0641 0.0231
-0.0004 0.0005 0.9993 0.0094 -0.0641 -0.0231
-1.9987 4.9976 3.9823 0.4193 0.0650 -0.7994
0.9990 -0.9992 0.0032 -0.1046 -0.0671 0.1293
0.9992 -0.0001 0.0003 -0.0471 -0.0048 -0.0201
-0.9992 0.0001 -0.0003 0.0471 0.0048 0.0201
-4.9954 -2.9981 -2.9910 0.0346 0.0292 0.6180

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54009
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.343
_diffrn_reflns_theta_min         2.951
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     16.00  52.00   1.00    1.00    --   42.33  57.00  60.00   36
  2  ω     55.00 111.00   1.00    1.00    --   42.33  57.00  60.00   56
  3  ω     83.00 111.00   1.00    2.50    --  111.00  61.00   0.00   28
  4  ω    112.00 178.00   1.00    2.50    --  111.00  77.00 -30.00   66
  5  ω    111.00 177.00   1.00    2.50    --  111.00  77.00 -90.00   66
  6  ω    117.00 145.00   1.00    2.50    --  111.00  61.00 -90.00   28
  7  ω    114.00 177.00   1.00    2.50    --  111.00  77.00-150.00   63
  8  ω    113.00 174.00   1.00    2.50    --  111.00  77.00-180.00   61
  9  ω     84.00 110.00   1.00    2.50    --  111.00  60.00-174.30   26
 10  ω     83.00 109.00   1.00    2.50    --  111.00  61.00-150.00   26
 11  ω     81.00 106.00   1.00    2.50    --  111.00  77.00-150.00   25
 12  ω     84.00 115.00   1.00    2.50    --  111.00  59.00-138.66   31
 13  ω     80.00 106.00   1.00    2.50    --  111.00  77.00 -90.00   26
 14  ω     83.00 109.00   1.00    2.50    --  111.00  61.00 -90.00   26
 15  ω     83.00 109.00   1.00    2.50    --  111.00  61.00 -60.00   26
 16  ω     83.00 109.00   1.00    2.50    --  111.00  61.00 -30.00   26
 17  ω    110.00 178.00   1.00    2.50    --  111.00  77.00   0.00   68
 18  ω    112.00 167.00   1.00    2.50    --  111.00  77.00  30.00   55
 19  ω    117.00 174.00   1.00    2.50    --  111.00  77.00  90.00   57
 20  ω     85.00 151.00   1.00    2.50    --  111.00  54.00 140.61   66
 21  ω     85.00 111.00   1.00    2.50    --  111.00  54.00 111.94   26
 22  ω     83.00 113.00   1.00    2.50    --  111.00  61.00 120.00   30
 23  ω     80.00 106.00   1.00    2.50    --  111.00  77.00  90.00   26
 24  ω     83.00 109.00   1.00    2.50    --  111.00  61.00  90.00   26
 25  ω     83.00 160.00   1.00    2.50    --  111.00  61.00  60.00   77
 26  ω     87.00 113.00   1.00    2.50    --  111.00  45.00  30.00   26
 27  ω     80.00 177.00   1.00    2.50    --  111.00  77.00  60.00   97
 28  ω     80.00 174.00   1.00    2.50    --  111.00  77.00 150.00   94
 29  ω     83.00 150.00   1.00    2.50    --  111.00  61.00 150.00   67
 30  ω     83.00 109.00   1.00    2.50    --  111.00  61.00  30.00   26
 31  ω     82.00 108.00   1.00    2.50    --  111.00  69.00  26.40   26
 32  ω     80.00 106.00   1.00    2.50    --  111.00  77.00   0.00   26
 33  ω     80.00 106.00   1.00    2.50    --  111.00  77.00 -30.00   26
 34  ω     80.00 150.00   1.00    2.50    --  111.00  77.00 -60.00   70
 35  ω     83.00 122.00   1.00    2.50    --  111.00  61.00-120.00   39
 36  ω     82.00 108.00   1.00    2.50    --  111.00  68.00 -61.97   26
 37  ω     80.00 176.00   1.00    2.50    --  111.00  77.00-120.00   96
 38  ω     80.00 106.00   1.00    2.50    --  111.00  77.00  30.00   26
 39  ω     80.00 106.00   1.00    2.50    --  111.00  77.00 120.00   26
 40  ω     23.00  68.00   1.00    1.00    --   42.33  38.00 -30.00   45
 41  ω      8.00 121.00   1.00    1.00    --   42.33  19.00-120.00  113
 42  ω     80.00 106.00   1.00    2.50    --  111.00  77.00-180.00   26
 43  ω     13.00 113.00   1.00    1.00    --   42.33  68.00 -18.86  100
 44  ω     42.00 114.00   1.00    2.50    --  111.00 -61.00-120.00   72
 45  ω     69.00 121.00   1.00    2.50    --  111.00-125.00 -30.00   52
 46  ω     62.00  95.00   1.00    2.50    --  111.00 -94.00-150.00   33
 47  ω     40.00 120.00   1.00    2.50    --  111.00-125.00-150.00   80
 48  ω     44.00 137.00   1.00    2.50    --  111.00 -77.00  30.00   93
 49  ω     66.00 119.00   1.00    2.50    --  111.00-125.00 120.00   53
 50  ω     60.00 117.00   1.00    1.00    --   42.33-178.00 120.00   57
 51  ω     30.00 102.00   1.00    2.50    --  111.00 -94.00   0.00   72
 52  ω      1.00  78.00   1.00    1.00    --   42.33 -99.00-150.00   77
 53  ω    -27.00  63.00   1.00    1.00    --   42.33 -57.00 -90.00   90
 54  ω    -44.00 -17.00   1.00    1.00    --  -42.33 -57.00-150.00   27
 55  ω    -71.00 -11.00   1.00    1.00    --  -42.33 -77.00-150.00   60
 56  ω    -59.00  26.00   1.00    1.00    --  -42.33  38.00 150.00   85
 57  ω    -64.00 -11.00   1.00    1.00    --  -42.33 -77.00  30.00   53
 58  ω    -84.00 -11.00   1.00    1.00    --  -42.33 -77.00 120.00   73
 59  ω    -81.00 -12.00   1.00    1.00    --  -42.33 -77.00 -30.00   69
 60  ω   -113.00 -97.00   1.00    1.00    --  -42.33 -77.00  30.00   16
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0470965000
_diffrn_orient_matrix_UB_12      0.0576490000
_diffrn_orient_matrix_UB_13      0.0093172000
_diffrn_orient_matrix_UB_21      -0.0047676000
_diffrn_orient_matrix_UB_22      0.0622192000
_diffrn_orient_matrix_UB_23      -0.0641611000
_diffrn_orient_matrix_UB_31      -0.0201121000
_diffrn_orient_matrix_UB_32      -0.1495998000
_diffrn_orient_matrix_UB_33      -0.0230852000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5801
_reflns_number_total             5945
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5945
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²+5.2333P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0795
_refine_special_details          ?
_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
Br1 Br 0.39804(2) 0.14532(2) 0.39064(2) 0.04563(7) Uani 1 1 d . . . . .
N1 N 0.39304(4) 0.44976(13) 0.56019(5) 0.0280(2) Uani 1 1 d . . . . .
N2 N 0.36773(4) 0.27889(13) 0.61648(5) 0.0271(2) Uani 1 1 d . . . . .
C1 C 0.37452(4) 0.42651(15) 0.61148(5) 0.0262(3) Uani 1 1 d . . . . .
C2 C 0.39767(5) 0.31423(17) 0.53194(6) 0.0334(3) Uani 1 1 d . . . . .
H2 H 0.409500 0.299231 0.495660 0.040 Uiso 1 1 calc R . . . .
C3 C 0.38182(5) 0.20779(16) 0.56683(6) 0.0335(3) Uani 1 1 d . . . . .
H3 H 0.380585 0.105833 0.559017 0.040 Uiso 1 1 calc R . . . .
C4 C 0.41208(4) 0.59180(16) 0.54383(6) 0.0290(3) Uani 1 1 d . . . . .
C5 C 0.45348(5) 0.63160(17) 0.57328(6) 0.0331(3) Uani 1 1 d . . . . .
C6 C 0.47107(5) 0.76943(19) 0.55876(7) 0.0419(3) Uani 1 1 d . . . . .
H6 H 0.498323 0.800560 0.577650 0.050 Uiso 1 1 calc R . . . .
C7 C 0.44830(6) 0.86027(19) 0.51645(9) 0.0467(4) Uani 1 1 d . . . . .
H7 H 0.460312 0.952405 0.507571 0.056 Uiso 1 1 calc R . . . .
C8 C 0.40815(5) 0.81645(19) 0.48730(8) 0.0425(4) Uani 1 1 d . . . . .
H8 H 0.393759 0.878636 0.458486 0.051 Uiso 1 1 calc R . . . .
C9 C 0.38869(5) 0.68033(17) 0.50024(6) 0.0338(3) Uani 1 1 d . . . . .
C10 C 0.48016(5) 0.52781(19) 0.61641(6) 0.0384(3) Uani 1 1 d . . . . .
H10 H 0.459834 0.451710 0.629586 0.046 Uiso 1 1 calc R . . . .
C11 C 0.50136(8) 0.6090(3) 0.67149(8) 0.0630(5) Uani 1 1 d . . . . .
H11A H 0.523221 0.678609 0.659854 0.095 Uiso 1 1 calc GR . . . .
H11B H 0.515515 0.537808 0.699008 0.095 Uiso 1 1 calc GR . . . .
H11C H 0.478708 0.661835 0.690319 0.095 Uiso 1 1 calc GR . . . .
C12 C 0.51590(8) 0.4495(3) 0.58432(9) 0.0735(7) Uani 1 1 d . . . . .
H12A H 0.502158 0.398299 0.549855 0.110 Uiso 1 1 calc GR . . . .
H12B H 0.531396 0.378779 0.610816 0.110 Uiso 1 1 calc GR . . . .
H12C H 0.536687 0.521989 0.572023 0.110 Uiso 1 1 calc GR . . . .
C13 C 0.34530(5) 0.63276(18) 0.46534(7) 0.0394(3) Uani 1 1 d . . . . .
H13 H 0.333351 0.546965 0.485714 0.047 Uiso 1 1 calc R . . . .
C14 C 0.31046(6) 0.7571(2) 0.46220(10) 0.0613(5) Uani 1 1 d . . . . .
H14A H 0.305838 0.789026 0.501897 0.092 Uiso 1 1 calc GR . . . .
H14B H 0.282859 0.720521 0.442638 0.092 Uiso 1 1 calc GR . . . .
H14C H 0.320768 0.839812 0.440096 0.092 Uiso 1 1 calc GR . . . .
C15 C 0.35426(7) 0.5839(3) 0.40221(8) 0.0582(5) Uani 1 1 d . . . . .
H15A H 0.368686 0.663587 0.382890 0.087 Uiso 1 1 calc GR . . . .
H15B H 0.326501 0.560097 0.379625 0.087 Uiso 1 1 calc GR . . . .
H15C H 0.373223 0.497487 0.404607 0.087 Uiso 1 1 calc GR . . . .
C16 C 0.34431(4) 0.21342(15) 0.66387(6) 0.0279(3) Uani 1 1 d . . . . .
C17 C 0.29769(5) 0.21530(16) 0.65632(6) 0.0333(3) Uani 1 1 d . . . . .
C18 C 0.27557(5) 0.1666(2) 0.70450(8) 0.0439(4) Uani 1 1 d . . . . .
H18 H 0.244526 0.165793 0.701389 0.053 Uiso 1 1 calc R . . . .
C19 C 0.29908(6) 0.1198(2) 0.75669(8) 0.0472(4) Uani 1 1 d . . . . .
H19 H 0.283668 0.091674 0.788861 0.057 Uiso 1 1 calc R . . . .
C20 C 0.34503(6) 0.11380(18) 0.76201(7) 0.0400(3) Uani 1 1 d . . . . .
H20 H 0.360168 0.078399 0.797146 0.048 Uiso 1 1 calc R . . . .
C21 C 0.36913(5) 0.16031(15) 0.71522(6) 0.0313(3) Uani 1 1 d . . . . .
C22 C 0.27150(5) 0.25987(19) 0.59822(7) 0.0404(3) Uani 1 1 d . . . . .
H22 H 0.292199 0.309716 0.573526 0.048 Uiso 1 1 calc R . . . .
C23 C 0.23406(9) 0.3680(4) 0.60691(12) 0.0923(10) Uani 1 1 d . . . . .
H23A H 0.211739 0.318953 0.627692 0.138 Uiso 1 1 calc GR . . . .
H23B H 0.220983 0.401721 0.568678 0.138 Uiso 1 1 calc GR . . . .
H23C H 0.245695 0.452052 0.629866 0.138 Uiso 1 1 calc GR . . . .
C24 C 0.25504(11) 0.1180(3) 0.56563(11) 0.0875(9) Uani 1 1 d . . . . .
H24A H 0.280184 0.058830 0.556698 0.131 Uiso 1 1 calc GR . . . .
H24B H 0.237627 0.144132 0.529161 0.131 Uiso 1 1 calc GR . . . .
H24C H 0.236954 0.061647 0.590551 0.131 Uiso 1 1 calc GR . . . .
C25 C 0.41974(5) 0.14774(17) 0.72038(7) 0.0368(3) Uani 1 1 d . . . . .
H25 H 0.431142 0.218855 0.692383 0.044 Uiso 1 1 calc R . . . .
C26 C 0.43340(6) -0.0091(2) 0.70267(10) 0.0587(5) Uani 1 1 d . . . . .
H26A H 0.423724 -0.080203 0.730683 0.088 Uiso 1 1 calc GR . . . .
H26B H 0.465291 -0.013842 0.702796 0.088 Uiso 1 1 calc GR . . . .
H26C H 0.419787 -0.031869 0.663398 0.088 Uiso 1 1 calc GR . . . .
C27 C 0.44053(6) 0.1860(2) 0.78327(8) 0.0532(4) Uani 1 1 d . . . . .
H27A H 0.428494 0.278784 0.795857 0.080 Uiso 1 1 calc GR . . . .
H27B H 0.472307 0.194859 0.782995 0.080 Uiso 1 1 calc GR . . . .
H27C H 0.433821 0.108181 0.810417 0.080 Uiso 1 1 calc GR . . . .
C28 C 0.36251(5) 0.53971(15) 0.65428(6) 0.0307(3) Uani 1 1 d . . . . .
C29 C 0.38102(6) 0.53362(18) 0.71301(7) 0.0425(4) Uani 1 1 d . . . . .
H29 H 0.402144 0.460864 0.724559 0.051 Uiso 1 1 calc R . . . .
C30 C 0.36829(7) 0.6350(2) 0.75459(8) 0.0540(5) Uani 1 1 d . . . . .
H30 H 0.380949 0.631053 0.793904 0.065 Uiso 1 1 calc R . . . .
C31 C 0.33700(7) 0.7411(2) 0.73758(9) 0.0582(5) Uani 1 1 d . . . . .
H31 H 0.327829 0.807665 0.765705 0.070 Uiso 1 1 calc R . . . .
C32 C 0.31890(8) 0.7501(2) 0.67900(11) 0.0656(6) Uani 1 1 d . . . . .
H32 H 0.298086 0.824006 0.667703 0.079 Uiso 1 1 calc R . . . .
C33 C 0.33168(7) 0.64906(19) 0.63675(9) 0.0496(4) Uani 1 1 d . . . . .
H33 H 0.319592 0.655135 0.597217 0.060 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.3436(16) . ?
N1 C2 1.3831(18) . ?
N1 C4 1.4565(17) . ?
N2 C1 1.3441(18) . ?
N2 C3 1.3858(17) . ?
N2 C16 1.4552(16) . ?
C1 C28 1.4663(18) . ?
C2 H2 0.9300 . ?
C2 C3 1.350(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(2) . ?
C4 C9 1.398(2) . ?
C5 C6 1.394(2) . ?
C5 C10 1.518(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.384(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.376(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.395(2) . ?
C9 C13 1.520(2) . ?
C10 H10 0.9800 . ?
C10 C11 1.524(2) . ?
C10 C12 1.521(2) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.526(2) . ?
C13 C15 1.534(2) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.3970(19) . ?
C16 C21 1.398(2) . ?
C17 C18 1.394(2) . ?
C17 C22 1.515(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.378(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.377(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.396(2) . ?
C21 C25 1.520(2) . ?
C22 H22 0.9800 . ?
C22 C23 1.512(3) . ?
C22 C24 1.526(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.527(2) . ?
C25 C27 1.531(2) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.386(2) . ?
C28 C33 1.381(2) . ?
C29 H29 0.9300 . ?
C29 C30 1.383(2) . ?
C30 H30 0.9300 . ?
C30 C31 1.366(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.380(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.392(3) . ?
C33 H33 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
C1 N1 C2 109.04(11) . . ?
C1 N1 C4 123.84(11) . . ?
C2 N1 C4 126.26(11) . . ?
C1 N2 C3 108.92(11) . . ?
C1 N2 C16 123.05(11) . . ?
C3 N2 C16 127.65(11) . . ?
N1 C1 N2 107.62(11) . . ?
N1 C1 C28 127.16(12) . . ?
N2 C1 C28 125.21(11) . . ?
N1 C2 H2 126.4 . . ?
C3 C2 N1 107.24(12) . . ?
C3 C2 H2 126.4 . . ?
N2 C3 H3 126.4 . . ?
C2 C3 N2 107.18(12) . . ?
C2 C3 H3 126.4 . . ?
C5 C4 N1 117.14(12) . . ?
C9 C4 N1 119.23(12) . . ?
C9 C4 C5 123.63(13) . . ?
C4 C5 C10 122.67(13) . . ?
C6 C5 C4 117.06(14) . . ?
C6 C5 C10 120.16(14) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.49(15) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 121.05(15) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.11(15) . . ?
C9 C8 H8 119.4 . . ?
C4 C9 C13 123.68(13) . . ?
C8 C9 C4 116.63(14) . . ?
C8 C9 C13 119.63(14) . . ?
C5 C10 H10 108.2 . . ?
C5 C10 C11 112.53(15) . . ?
C5 C10 C12 109.51(12) . . ?
C11 C10 H10 108.2 . . ?
C12 C10 H10 108.2 . . ?
C12 C10 C11 110.20(16) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 108.3 . . ?
C9 C13 C14 111.86(15) . . ?
C9 C13 C15 109.93(13) . . ?
C14 C13 H13 108.3 . . ?
C14 C13 C15 110.18(15) . . ?
C15 C13 H13 108.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 117.11(12) . . ?
C17 C16 C21 123.83(12) . . ?
C21 C16 N2 118.96(12) . . ?
C16 C17 C22 122.90(13) . . ?
C18 C17 C16 116.67(14) . . ?
C18 C17 C22 120.36(14) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.88(15) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.11(14) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.72(15) . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C25 122.80(13) . . ?
C20 C21 C16 116.68(13) . . ?
C20 C21 C25 120.49(13) . . ?
C17 C22 H22 107.6 . . ?
C17 C22 C24 108.29(15) . . ?
C23 C22 C17 113.00(15) . . ?
C23 C22 H22 107.6 . . ?
C23 C22 C24 112.5(2) . . ?
C24 C22 H22 107.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 108.1 . . ?
C21 C25 C26 109.90(13) . . ?
C21 C25 C27 111.93(14) . . ?
C26 C25 H25 108.1 . . ?
C26 C25 C27 110.49(15) . . ?
C27 C25 H25 108.1 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 119.79(13) . . ?
C33 C28 C1 120.21(14) . . ?
C33 C28 C29 119.95(14) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.44(17) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 120.2 . . ?
C31 C30 C29 119.63(18) . . ?
C31 C30 H30 120.2 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.53(16) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 119.9 . . ?
C31 C32 C33 120.27(19) . . ?
C33 C32 H32 119.9 . . ?
C28 C33 C32 119.16(18) . . ?
C28 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C28 C29 -121.62(16) . . . . ?
N1 C1 C28 C33 60.7(2) . . . . ?
N1 C2 C3 N2 -0.26(16) . . . . ?
N1 C4 C5 C6 -178.28(12) . . . . ?
N1 C4 C5 C10 5.45(19) . . . . ?
N1 C4 C9 C8 178.76(13) . . . . ?
N1 C4 C9 C13 -4.1(2) . . . . ?
N2 C1 C28 C29 60.0(2) . . . . ?
N2 C1 C28 C33 -117.69(17) . . . . ?
N2 C16 C17 C18 -173.54(13) . . . . ?
N2 C16 C17 C22 9.5(2) . . . . ?
N2 C16 C21 C20 173.15(13) . . . . ?
N2 C16 C21 C25 -8.8(2) . . . . ?
C1 N1 C2 C3 -0.17(16) . . . . ?
C1 N1 C4 C5 74.41(17) . . . . ?
C1 N1 C4 C9 -105.68(15) . . . . ?
C1 N2 C3 C2 0.61(16) . . . . ?
C1 N2 C16 C17 81.37(16) . . . . ?
C1 N2 C16 C21 -95.16(16) . . . . ?
C1 C28 C29 C30 -176.67(15) . . . . ?
C1 C28 C33 C32 176.33(17) . . . . ?
C2 N1 C1 N2 0.55(15) . . . . ?
C2 N1 C1 C28 -178.04(13) . . . . ?
C2 N1 C4 C5 -93.77(16) . . . . ?
C2 N1 C4 C9 86.13(18) . . . . ?
C3 N2 C1 N1 -0.72(15) . . . . ?
C3 N2 C1 C28 177.91(13) . . . . ?
C3 N2 C16 C17 -90.70(17) . . . . ?
C3 N2 C16 C21 92.76(17) . . . . ?
C4 N1 C1 N2 -169.39(12) . . . . ?
C4 N1 C1 C28 12.0(2) . . . . ?
C4 N1 C2 C3 169.47(13) . . . . ?
C4 C5 C6 C7 -0.8(2) . . . . ?
C4 C5 C10 C11 -138.77(16) . . . . ?
C4 C5 C10 C12 98.31(19) . . . . ?
C4 C9 C13 C14 134.13(16) . . . . ?
C4 C9 C13 C15 -103.12(18) . . . . ?
C5 C4 C9 C8 -1.3(2) . . . . ?
C5 C4 C9 C13 175.80(14) . . . . ?
C5 C6 C7 C8 -0.7(3) . . . . ?
C6 C5 C10 C11 45.1(2) . . . . ?
C6 C5 C10 C12 -77.9(2) . . . . ?
C6 C7 C8 C9 1.2(3) . . . . ?
C7 C8 C9 C4 -0.2(2) . . . . ?
C7 C8 C9 C13 -177.48(16) . . . . ?
C8 C9 C13 C14 -48.8(2) . . . . ?
C8 C9 C13 C15 73.94(19) . . . . ?
C9 C4 C5 C6 1.8(2) . . . . ?
C9 C4 C5 C10 -174.45(13) . . . . ?
C10 C5 C6 C7 175.61(15) . . . . ?
C16 N2 C1 N1 -174.09(11) . . . . ?
C16 N2 C1 C28 4.5(2) . . . . ?
C16 N2 C3 C2 173.59(13) . . . . ?
C16 C17 C18 C19 0.2(2) . . . . ?
C16 C17 C22 C23 -133.4(2) . . . . ?
C16 C17 C22 C24 101.2(2) . . . . ?
C16 C21 C25 C26 -93.56(18) . . . . ?
C16 C21 C25 C27 143.27(15) . . . . ?
C17 C16 C21 C20 -3.1(2) . . . . ?
C17 C16 C21 C25 174.89(13) . . . . ?
C17 C18 C19 C20 -2.7(3) . . . . ?
C18 C17 C22 C23 49.7(2) . . . . ?
C18 C17 C22 C24 -75.7(2) . . . . ?
C18 C19 C20 C21 2.3(3) . . . . ?
C19 C20 C21 C16 0.5(2) . . . . ?
C19 C20 C21 C25 -177.56(15) . . . . ?
C20 C21 C25 C26 84.40(19) . . . . ?
C20 C21 C25 C27 -38.8(2) . . . . ?
C21 C16 C17 C18 2.8(2) . . . . ?
C21 C16 C17 C22 -174.16(14) . . . . ?
C22 C17 C18 C19 177.20(16) . . . . ?
C28 C29 C30 C31 0.5(3) . . . . ?
C29 C28 C33 C32 -1.4(3) . . . . ?
C29 C30 C31 C32 -1.7(3) . . . . ?
C30 C31 C32 C33 1.3(3) . . . . ?
C31 C32 C33 C28 0.2(3) . . . . ?
C33 C28 C29 C30 1.0(2) . . . . ?

_olex2_date_sample_data_collection 2017-01-20
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.830
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
####################################################################### 
# 
# 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_compound_3j
_database_code_depnum_ccdc_archive 'CCDC 1559109'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;


_audit_creation_date             2017-05-19
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'Br, C35 H46 N3'
_chemical_formula_sum            'C35 H46 Br N3'
_chemical_formula_weight         588.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C35 H46 N3 Br'
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'
Br Br -0.2901 2.4595 '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 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                   9.07979(11)
_cell_length_b                   26.6494(4)
_cell_length_c                   13.52664(16)
_cell_angle_alpha                90
_cell_angle_beta                 95.0975(11)
_cell_angle_gamma                90
_cell_volume                     3260.11(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    59052
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.6750
_cell_measurement_theta_min      2.1480
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1248
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 -2 0.0843
1 5 -2 0.0939
-5 4 -3 0.0521
-1 -5 2 0.0939
0 3 -5 0.0854
0 -3 5 0.0854
5 1 -5 0.0523
-1 5 -2 0.0623
1 -5 2 0.0623
0 5 2 0.0843

_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.125
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0023 -4.9953 -1.9971 0.1501 0.0460 0.0640
0.9986 4.9883 -1.9987 -0.0767 -0.0967 0.1347
-4.9907 4.0519 -2.9911 -0.1577 0.3702 0.1965
-0.9986 -4.9883 1.9987 0.0767 0.0967 -0.1347
-0.0014 3.0024 -4.9936 -0.0070 0.0112 0.2744
0.0014 -3.0024 4.9936 0.0070 -0.0112 -0.2744
4.9885 0.9518 -4.9986 0.1416 -0.3537 0.2440
-0.9976 5.0090 -1.9966 -0.1164 0.0546 0.1409
0.9976 -5.0090 1.9966 0.1164 -0.0546 -0.1409
0.0023 4.9953 1.9971 -0.1501 -0.0460 -0.0640

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            188113
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         1.528
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9665
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  96.00   1.00   27.50    --   25.97  77.00-120.00  100
  2  ω    -43.00  47.00   1.00   27.50    --   25.97 -57.00 120.00   90
  3  ω    -44.00  56.00   1.00   27.50    --   25.97 -77.00  30.00  100
  4  ω      6.00  95.00   1.00   27.50    --   25.97  57.00  90.00   89
  5  ω      6.00  95.00   1.00   27.50    --   25.97  57.00   0.00   89
  6  ω    -20.00  68.00   1.00   27.50    --   25.97 -99.00  90.00   88
  7  ω     -4.00  96.00   1.00   27.50    --   25.97  77.00 150.00  100
  8  ω    -44.00  56.00   1.00   27.50    --   25.97 -77.00 -60.00  100
  9  ω     -4.00  96.00   1.00   27.50    --   25.97  77.00   0.00  100
 10  ω    -20.00  68.00   1.00   27.50    --   25.97 -99.00-120.00   88
 11  ω    -99.00 -35.00   1.00   27.50    --  -23.50-178.00 120.00   64
 12  ω     -4.00  96.00   1.00   27.50    --   25.97  77.00  30.00  100
 13  ω    -17.00  70.00   1.00   27.50    --   25.97-103.00 -35.00   87
 14  ω    -47.00  99.00   1.00   27.50    --   25.97   0.00-150.00  146
 15  ω      6.00  95.00   1.00   27.50    --   25.97  57.00 -60.00   89
 16  ω     34.00 103.00   1.00   27.50    --   25.97-178.00-120.00   69
 17  ω    -20.00  68.00   1.00   27.50    --   25.97 -99.00  60.00   88
 18  ω    -47.00  99.00   1.00   27.50    --   25.97   0.00-180.00  146
 19  ω    -46.00  51.00   1.00   27.50    --   25.97 -38.00 -90.00   97
 20  ω      0.00  98.00   1.00   27.50    --   25.97  38.00 -60.00   98
 21  ω    -47.00  99.00   1.00   27.50    --   25.97   0.00 -90.00  146
 22  ω    -47.00  99.00   1.00   27.50    --   25.97   0.00 -60.00  146
 23  ω    -47.00  33.00   1.00   27.50    --   25.97   0.00 -30.00   80
 24  ω    -47.00  99.00   1.00   27.50    --   25.97   0.00-120.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0196128000
_diffrn_orient_matrix_UB_12      -0.0246869000
_diffrn_orient_matrix_UB_13      -0.0134469000
_diffrn_orient_matrix_UB_21      -0.0758730000
_diffrn_orient_matrix_UB_22      -0.0066855000
_diffrn_orient_matrix_UB_23      -0.0062309000
_diffrn_orient_matrix_UB_31      -0.0031077000
_diffrn_orient_matrix_UB_32      0.0073805000
_diffrn_orient_matrix_UB_33      -0.0505079000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8750
_reflns_number_total             9564
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         9564
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0270P)²+2.1497P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0722
_refine_special_details          
;
 ?
;
_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
Br1 Br 0.93313(2) 0.37757(2) 0.09376(2) 0.01795(4) Uani 1 1 d . . . . .
N1 N 0.71000(11) 0.36370(4) 0.75826(7) 0.01406(18) Uani 1 1 d . . . . .
N2 N 0.54688(11) 0.41220(4) 0.81692(7) 0.01334(18) Uani 1 1 d . . . . .
N3 N 0.23015(13) 0.38108(4) 0.36724(8) 0.0197(2) Uani 1 1 d . . . . .
C1 C 0.57825(12) 0.38616(4) 0.73559(8) 0.0126(2) Uani 1 1 d . . . . .
C2 C 0.76234(13) 0.37556(5) 0.85475(9) 0.0170(2) Uani 1 1 d . . . . .
H2 H 0.8507 0.3648 0.8880 0.020 Uiso 1 1 calc R U . . .
C3 C 0.66060(13) 0.40574(5) 0.89134(9) 0.0165(2) Uani 1 1 d . . . . .
H3 H 0.6658 0.4196 0.9547 0.020 Uiso 1 1 calc R U . . .
C4 C 0.79563(13) 0.33400(5) 0.69422(9) 0.0153(2) Uani 1 1 d . . . . .
C5 C 0.88194(14) 0.35909(5) 0.62964(9) 0.0176(2) Uani 1 1 d . . . . .
C6 C 0.97646(15) 0.32975(6) 0.57741(10) 0.0228(3) Uani 1 1 d . . . . .
H6 H 1.0356 0.3450 0.5334 0.027 Uiso 1 1 calc R U . . .
C7 C 0.98294(16) 0.27820(6) 0.59047(11) 0.0254(3) Uani 1 1 d . . . . .
H7 H 1.0486 0.2594 0.5566 0.031 Uiso 1 1 calc R U . . .
C8 C 0.89305(15) 0.25442(5) 0.65316(11) 0.0238(3) Uani 1 1 d . . . . .
H8 H 0.8974 0.2197 0.6598 0.029 Uiso 1 1 calc R U . . .
C9 C 0.79589(14) 0.28181(5) 0.70660(10) 0.0188(2) Uani 1 1 d . . . . .
C10 C 0.87485(15) 0.41544(5) 0.61298(10) 0.0211(2) Uani 1 1 d . . . . .
H10 H 0.8101 0.4299 0.6598 0.025 Uiso 1 1 calc R U . . .
C11 C 0.80719(17) 0.42655(6) 0.50758(12) 0.0309(3) Uani 1 1 d . . . . .
H11A H 0.8661 0.4111 0.4605 0.046 Uiso 1 1 calc R U . . .
H11B H 0.8046 0.4622 0.4970 0.046 Uiso 1 1 calc R U . . .
H11C H 0.7085 0.4134 0.4991 0.046 Uiso 1 1 calc R U . . .
C12 C 1.02762(17) 0.43966(6) 0.63219(12) 0.0290(3) Uani 1 1 d . . . . .
H12A H 1.0683 0.4318 0.6983 0.044 Uiso 1 1 calc R U . . .
H12B H 1.0186 0.4754 0.6250 0.044 Uiso 1 1 calc R U . . .
H12C H 1.0918 0.4270 0.5853 0.044 Uiso 1 1 calc R U . . .
C13 C 0.69743(15) 0.25521(5) 0.77509(11) 0.0243(3) Uani 1 1 d . . . . .
H13 H 0.6222 0.2791 0.7929 0.029 Uiso 1 1 calc R U . . .
C14 C 0.61763(19) 0.21025(6) 0.72416(15) 0.0374(4) Uani 1 1 d . . . . .
H14A H 0.5600 0.2213 0.6653 0.056 Uiso 1 1 calc R U . . .
H14B H 0.5537 0.1952 0.7686 0.056 Uiso 1 1 calc R U . . .
H14C H 0.6892 0.1860 0.7066 0.056 Uiso 1 1 calc R U . . .
C15 C 0.7864(2) 0.23858(7) 0.87092(14) 0.0405(4) Uani 1 1 d . . . . .
H15A H 0.8604 0.2148 0.8555 0.061 Uiso 1 1 calc R U . . .
H15B H 0.7213 0.2233 0.9143 0.061 Uiso 1 1 calc R U . . .
H15C H 0.8333 0.2672 0.9031 0.061 Uiso 1 1 calc R U . . .
C16 C 0.40528(12) 0.43324(4) 0.83737(8) 0.0133(2) Uani 1 1 d . . . . .
C17 C 0.30214(13) 0.40035(5) 0.87384(9) 0.0155(2) Uani 1 1 d . . . . .
C18 C 0.17244(14) 0.42164(5) 0.90345(10) 0.0195(2) Uani 1 1 d . . . . .
H18 H 0.1021 0.4012 0.9291 0.023 Uiso 1 1 calc R U . . .
C19 C 0.14742(14) 0.47271(5) 0.89503(10) 0.0219(3) Uani 1 1 d . . . . .
H19 H 0.0600 0.4861 0.9146 0.026 Uiso 1 1 calc R U . . .
C20 C 0.25074(15) 0.50421(5) 0.85788(10) 0.0199(2) Uani 1 1 d . . . . .
H20 H 0.2313 0.5384 0.8520 0.024 Uiso 1 1 calc R U . . .
C21 C 0.38373(13) 0.48518(5) 0.82918(8) 0.0151(2) Uani 1 1 d . . . . .
C22 C 0.32744(15) 0.34406(5) 0.88315(10) 0.0201(2) Uani 1 1 d . . . . .
H22 H 0.4223 0.3365 0.8571 0.024 Uiso 1 1 calc R U . . .
C23 C 0.2085(3) 0.31536(7) 0.8216(2) 0.0650(8) Uani 1 1 d . . . . .
H23A H 0.1154 0.3200 0.8490 0.097 Uiso 1 1 calc R U . . .
H23B H 0.2331 0.2803 0.8223 0.097 Uiso 1 1 calc R U . . .
H23C H 0.2014 0.3276 0.7546 0.097 Uiso 1 1 calc R U . . .
C24 C 0.3370(3) 0.32701(7) 0.99061(14) 0.0512(6) Uani 1 1 d . . . . .
H24A H 0.4187 0.3434 1.0272 0.077 Uiso 1 1 calc R U . . .
H24B H 0.3514 0.2913 0.9936 0.077 Uiso 1 1 calc R U . . .
H24C H 0.2470 0.3355 1.0189 0.077 Uiso 1 1 calc R U . . .
C25 C 0.50097(15) 0.52057(5) 0.79590(9) 0.0180(2) Uani 1 1 d . . . . .
H25 H 0.5710 0.5007 0.7610 0.022 Uiso 1 1 calc R U . . .
C26 C 0.4346(2) 0.56074(6) 0.72460(12) 0.0327(3) Uani 1 1 d . . . . .
H26A H 0.3798 0.5449 0.6692 0.049 Uiso 1 1 calc R U . . .
H26B H 0.5126 0.5807 0.7013 0.049 Uiso 1 1 calc R U . . .
H26C H 0.3698 0.5819 0.7585 0.049 Uiso 1 1 calc R U . . .
C27 C 0.5861(2) 0.54499(7) 0.88595(11) 0.0377(4) Uani 1 1 d . . . . .
H27A H 0.5202 0.5656 0.9201 0.057 Uiso 1 1 calc R U . . .
H27B H 0.6644 0.5654 0.8643 0.057 Uiso 1 1 calc R U . . .
H27C H 0.6273 0.5194 0.9300 0.057 Uiso 1 1 calc R U . . .
C28 C 0.48958(12) 0.38435(4) 0.64034(9) 0.0133(2) Uani 1 1 d . . . . .
C29 C 0.43344(13) 0.42853(5) 0.59566(9) 0.0154(2) Uani 1 1 d . . . . .
H29 H 0.4514 0.4590 0.6279 0.019 Uiso 1 1 calc R U . . .
C30 C 0.35186(14) 0.42774(5) 0.50454(9) 0.0164(2) Uani 1 1 d . . . . .
H30 H 0.3184 0.4578 0.4757 0.020 Uiso 1 1 calc R U . . .
C31 C 0.31834(13) 0.38208(5) 0.45433(9) 0.0151(2) Uani 1 1 d . . . . .
C32 C 0.37914(14) 0.33774(5) 0.49859(9) 0.0177(2) Uani 1 1 d . . . . .
H32 H 0.3626 0.3072 0.4663 0.021 Uiso 1 1 calc R U . . .
C33 C 0.46289(13) 0.33909(5) 0.58920(9) 0.0167(2) Uani 1 1 d . . . . .
H33 H 0.5021 0.3094 0.6166 0.020 Uiso 1 1 calc R U . . .
C34 C 0.15737(15) 0.42665(5) 0.32859(10) 0.0215(2) Uani 1 1 d . . . . .
H34A H 0.0997 0.4407 0.3779 0.032 Uiso 1 1 calc R U . . .
H34B H 0.0938 0.4188 0.2701 0.032 Uiso 1 1 calc R U . . .
H34C H 0.2306 0.4505 0.3122 0.032 Uiso 1 1 calc R U . . .
C35 C 0.19620(16) 0.33390(5) 0.31635(10) 0.0232(3) Uani 1 1 d . . . . .
H35A H 0.2863 0.3183 0.3002 0.035 Uiso 1 1 calc R U . . .
H35B H 0.1339 0.3402 0.2565 0.035 Uiso 1 1 calc R U . . .
H35C H 0.1459 0.3121 0.3587 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.3484(15) . ?
N1 C2 1.3853(15) . ?
N1 C4 1.4496(15) . ?
N2 C1 1.3523(14) . ?
N2 C3 1.3872(15) . ?
N2 C16 1.4516(14) . ?
N3 C31 1.3645(15) . ?
N3 C34 1.4572(17) . ?
N3 C35 1.4532(17) . ?
C1 C28 1.4581(16) . ?
C2 H2 0.9300 . ?
C2 C3 1.3514(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.3950(18) . ?
C4 C9 1.4007(17) . ?
C5 C6 1.3982(17) . ?
C5 C10 1.5189(18) . ?
C6 H6 0.9300 . ?
C6 C7 1.386(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.382(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.3953(18) . ?
C9 C13 1.5191(19) . ?
C10 H10 0.9800 . ?
C10 C11 1.530(2) . ?
C10 C12 1.531(2) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.532(2) . ?
C13 C15 1.531(2) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.4039(16) . ?
C16 C21 1.4008(16) . ?
C17 C18 1.3975(17) . ?
C17 C22 1.5210(18) . ?
C18 H18 0.9300 . ?
C18 C19 1.3829(19) . ?
C19 H19 0.9300 . ?
C19 C20 1.3860(19) . ?
C20 H20 0.9300 . ?
C20 C21 1.3963(17) . ?
C21 C25 1.5201(17) . ?
C22 H22 0.9800 . ?
C22 C23 1.511(2) . ?
C22 C24 1.518(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.5283(19) . ?
C25 C27 1.5289(19) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.3989(16) . ?
C28 C33 1.4008(16) . ?
C29 H29 0.9300 . ?
C29 C30 1.3805(16) . ?
C30 H30 0.9300 . ?
C30 C31 1.4134(17) . ?
C31 C32 1.4146(17) . ?
C32 H32 0.9300 . ?
C32 C33 1.3842(17) . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 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
C1 N1 C2 109.65(10) . . ?
C1 N1 C4 128.21(10) . . ?
C2 N1 C4 122.03(10) . . ?
C1 N2 C3 109.24(10) . . ?
C1 N2 C16 127.40(10) . . ?
C3 N2 C16 121.63(10) . . ?
C31 N3 C34 120.40(11) . . ?
C31 N3 C35 120.62(11) . . ?
C35 N3 C34 118.73(10) . . ?
N1 C1 N2 106.83(10) . . ?
N1 C1 C28 126.54(10) . . ?
N2 C1 C28 126.60(10) . . ?
N1 C2 H2 126.5 . . ?
C3 C2 N1 107.00(10) . . ?
C3 C2 H2 126.5 . . ?
N2 C3 H3 126.4 . . ?
C2 C3 N2 107.29(10) . . ?
C2 C3 H3 126.4 . . ?
C5 C4 N1 118.25(11) . . ?
C5 C4 C9 123.76(11) . . ?
C9 C4 N1 117.78(11) . . ?
C4 C5 C6 116.90(12) . . ?
C4 C5 C10 123.24(11) . . ?
C6 C5 C10 119.85(12) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.74(13) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.80(13) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.87(13) . . ?
C9 C8 H8 119.6 . . ?
C4 C9 C13 122.79(12) . . ?
C8 C9 C4 116.87(12) . . ?
C8 C9 C13 120.34(12) . . ?
C5 C10 H10 108.2 . . ?
C5 C10 C11 109.74(12) . . ?
C5 C10 C12 111.46(11) . . ?
C11 C10 H10 108.2 . . ?
C11 C10 C12 111.05(12) . . ?
C12 C10 H10 108.2 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 107.9 . . ?
C9 C13 C14 111.80(13) . . ?
C9 C13 C15 110.90(12) . . ?
C14 C13 H13 107.9 . . ?
C15 C13 H13 107.9 . . ?
C15 C13 C14 110.33(13) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 117.10(10) . . ?
C21 C16 N2 119.11(10) . . ?
C21 C16 C17 123.49(11) . . ?
C16 C17 C22 122.98(11) . . ?
C18 C17 C16 116.91(11) . . ?
C18 C17 C22 120.10(11) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.83(12) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.5 . . ?
C18 C19 C20 120.95(12) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.71(12) . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C25 122.68(11) . . ?
C20 C21 C16 117.07(11) . . ?
C20 C21 C25 120.17(11) . . ?
C17 C22 H22 107.8 . . ?
C23 C22 C17 111.00(12) . . ?
C23 C22 H22 107.8 . . ?
C23 C22 C24 110.67(17) . . ?
C24 C22 C17 111.70(12) . . ?
C24 C22 H22 107.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 108.0 . . ?
C21 C25 C26 111.98(12) . . ?
C21 C25 C27 110.25(10) . . ?
C26 C25 H25 108.0 . . ?
C26 C25 C27 110.35(13) . . ?
C27 C25 H25 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 120.35(10) . . ?
C29 C28 C33 118.09(11) . . ?
C33 C28 C1 121.51(10) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 C28 121.26(11) . . ?
C30 C29 H29 119.4 . . ?
C29 C30 H30 119.4 . . ?
C29 C30 C31 121.18(11) . . ?
C31 C30 H30 119.4 . . ?
N3 C31 C30 121.10(11) . . ?
N3 C31 C32 121.74(11) . . ?
C30 C31 C32 117.16(11) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 C31 121.06(11) . . ?
C33 C32 H32 119.5 . . ?
C28 C33 H33 119.4 . . ?
C32 C33 C28 121.14(11) . . ?
C32 C33 H33 119.4 . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
N3 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C35 H35A 109.5 . . ?
N3 C35 H35B 109.5 . . ?
N3 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C28 C29 -130.79(13) . . . . ?
N1 C1 C28 C33 46.68(18) . . . . ?
N1 C2 C3 N2 -0.12(14) . . . . ?
N1 C4 C5 C6 172.66(11) . . . . ?
N1 C4 C5 C10 -8.57(18) . . . . ?
N1 C4 C9 C8 -172.24(11) . . . . ?
N1 C4 C9 C13 7.22(17) . . . . ?
N2 C1 C28 C29 46.53(17) . . . . ?
N2 C1 C28 C33 -136.00(13) . . . . ?
N2 C16 C17 C18 173.34(10) . . . . ?
N2 C16 C17 C22 -5.82(17) . . . . ?
N2 C16 C21 C20 -174.55(10) . . . . ?
N2 C16 C21 C25 2.32(17) . . . . ?
N3 C31 C32 C33 -177.03(12) . . . . ?
C1 N1 C2 C3 0.02(14) . . . . ?
C1 N1 C4 C5 80.72(16) . . . . ?
C1 N1 C4 C9 -104.30(14) . . . . ?
C1 N2 C3 C2 0.17(14) . . . . ?
C1 N2 C16 C17 80.56(15) . . . . ?
C1 N2 C16 C21 -105.48(14) . . . . ?
C1 C28 C29 C30 178.63(11) . . . . ?
C1 C28 C33 C32 -179.70(11) . . . . ?
C2 N1 C1 N2 0.08(13) . . . . ?
C2 N1 C1 C28 177.83(11) . . . . ?
C2 N1 C4 C5 -94.97(14) . . . . ?
C2 N1 C4 C9 80.02(15) . . . . ?
C3 N2 C1 N1 -0.16(13) . . . . ?
C3 N2 C1 C28 -177.90(11) . . . . ?
C3 N2 C16 C17 -82.82(14) . . . . ?
C3 N2 C16 C21 91.14(14) . . . . ?
C4 N1 C1 N2 -176.03(11) . . . . ?
C4 N1 C1 C28 1.7(2) . . . . ?
C4 N1 C2 C3 176.43(11) . . . . ?
C4 C5 C6 C7 -0.23(19) . . . . ?
C4 C5 C10 C11 -111.59(14) . . . . ?
C4 C5 C10 C12 124.98(13) . . . . ?
C4 C9 C13 C14 132.36(13) . . . . ?
C4 C9 C13 C15 -104.05(16) . . . . ?
C5 C4 C9 C8 2.44(18) . . . . ?
C5 C4 C9 C13 -178.10(12) . . . . ?
C5 C6 C7 C8 1.9(2) . . . . ?
C6 C5 C10 C11 67.15(16) . . . . ?
C6 C5 C10 C12 -56.28(16) . . . . ?
C6 C7 C8 C9 -1.4(2) . . . . ?
C7 C8 C9 C4 -0.66(19) . . . . ?
C7 C8 C9 C13 179.86(13) . . . . ?
C8 C9 C13 C14 -48.19(17) . . . . ?
C8 C9 C13 C15 75.40(17) . . . . ?
C9 C4 C5 C6 -2.00(18) . . . . ?
C9 C4 C5 C10 176.77(12) . . . . ?
C10 C5 C6 C7 -179.05(13) . . . . ?
C16 N2 C1 N1 -165.21(11) . . . . ?
C16 N2 C1 C28 17.04(19) . . . . ?
C16 N2 C3 C2 166.25(11) . . . . ?
C16 C17 C18 C19 1.13(18) . . . . ?
C16 C17 C22 C23 -120.20(18) . . . . ?
C16 C17 C22 C24 115.77(16) . . . . ?
C16 C21 C25 C26 138.47(13) . . . . ?
C16 C21 C25 C27 -98.25(15) . . . . ?
C17 C16 C21 C20 -1.00(18) . . . . ?
C17 C16 C21 C25 175.87(11) . . . . ?
C17 C18 C19 C20 -0.6(2) . . . . ?
C18 C17 C22 C23 60.7(2) . . . . ?
C18 C17 C22 C24 -63.36(18) . . . . ?
C18 C19 C20 C21 -0.8(2) . . . . ?
C19 C20 C21 C16 1.57(18) . . . . ?
C19 C20 C21 C25 -175.38(12) . . . . ?
C20 C21 C25 C26 -44.76(16) . . . . ?
C20 C21 C25 C27 78.52(16) . . . . ?
C21 C16 C17 C18 -0.33(18) . . . . ?
C21 C16 C17 C22 -179.49(11) . . . . ?
C22 C17 C18 C19 -179.69(12) . . . . ?
C28 C29 C30 C31 1.88(19) . . . . ?
C29 C28 C33 C32 -2.17(18) . . . . ?
C29 C30 C31 N3 175.93(12) . . . . ?
C29 C30 C31 C32 -3.61(18) . . . . ?
C30 C31 C32 C33 2.51(18) . . . . ?
C31 C32 C33 C28 0.35(19) . . . . ?
C33 C28 C29 C30 1.07(18) . . . . ?
C34 N3 C31 C30 -5.64(19) . . . . ?
C34 N3 C31 C32 173.89(12) . . . . ?
C35 N3 C31 C30 -179.88(12) . . . . ?
C35 N3 C31 C32 -0.36(19) . . . . ?

_olex2_date_sample_data_collection 2017-04-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_compound_14
_database_code_depnum_ccdc_archive 'CCDC 1559110'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;


_audit_creation_date             2017-02-01
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C34 H43 N2), Br4 Ni [+ solvent]'
_chemical_formula_sum            'C68 H86 Br4 N4 Ni'
_chemical_formula_weight         1337.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C75 H94 Br4 N4 Ni'
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'
Br Br -0.2901 2.4595 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   22.2529(4)
_cell_length_b                   17.8637(4)
_cell_length_c                   18.7897(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.2084(18)
_cell_angle_gamma                90
_cell_volume                     7271.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17399
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      29.0840
_cell_measurement_theta_min      1.8770
_exptl_absorpt_coefficient_mu    2.502
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2760
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.0096
-1 0 -1 0.0096
-1 0 1 0.0572
1 0 -1 0.0572
-4 5 -2 0.1010
4 -5 2 0.1010
-3 -2 5 0.0636
5 -1 -2 0.0626
-5 1 2 0.0626

_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.019
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9990 -0.0004 0.9995 -0.0002 0.0454 0.0330
-0.9990 0.0004 -0.9995 0.0002 -0.0454 -0.0330
-0.9999 -0.0002 0.9997 -0.0382 0.0190 -0.0133
0.9999 0.0002 -0.9997 0.0382 -0.0190 0.0133
-3.9977 5.0002 -1.9978 0.0613 -0.0156 -0.2513
3.9977 -5.0002 1.9978 -0.0613 0.0156 0.2513
-3.0003 -2.0010 4.9979 -0.1924 0.0808 0.0355
4.9984 -0.9997 -2.0000 0.1135 -0.0187 0.1238
-4.9984 0.9997 2.0000 -0.1135 0.0187 -0.1238

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            83727
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         1.59
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.7909
_diffrn_measured_fraction_theta_max 0.9982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  94.00   1.00   33.00    --   24.94  77.00 120.00   98
  2  ω      6.00  93.00   1.00   33.00    --   24.94  57.00  90.00   87
  3  ω    -44.00  54.00   1.00   33.00    --   24.94 -77.00   0.00   98
  4  ω    -44.00  54.00   1.00   33.00    --   24.94 -77.00-180.00   98
  5  ω     -4.00  94.00   1.00   33.00    --   24.94  77.00-150.00   98
  6  ω     -4.00  94.00   1.00   33.00    --   24.94  77.00  30.00   98
  7  ω    -20.00  65.00   1.00   33.00    --   24.94 -99.00 -60.00   85
  8  ω    -46.00  47.00   1.00   33.00    --   24.94 -38.00  60.00   93
  9  ω     -4.00  94.00   1.00   33.00    --   24.94  77.00 -60.00   98
 10  ω      7.00  85.00   1.00   33.00    --   24.94-133.00 145.75   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0189987000
_diffrn_orient_matrix_UB_12      0.0197862000
_diffrn_orient_matrix_UB_13      -0.0191705000
_diffrn_orient_matrix_UB_21      0.0132085000
_diffrn_orient_matrix_UB_22      0.0203056000
_diffrn_orient_matrix_UB_23      0.0322243000
_diffrn_orient_matrix_UB_31      0.0231582000
_diffrn_orient_matrix_UB_32      -0.0278070000
_diffrn_orient_matrix_UB_33      0.0098754000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8207
_reflns_number_total             10702
_reflns_odcompleteness_completeness 79.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.78
_reflns_special_details          
;

 Disordered toluene was squeezed with the Olex routine. The sum formular 
 disregard the solvent.

Miller array info: D:\Data\kim03\struct\olex2_kim03\kim03.hkl:Iobs,SigIobs
Observation type: xray.intensity
Type of data: double, size=83727
Type of sigmas: double, size=83727
Number of Miller indices: 83727
Anomalous flag: False
Unit cell: (22.2529, 17.8637, 18.7897, 90, 103.208, 90)
Space group: I 1 2/a 1 (No. 15)
Systematic absences: 1442
Systematic absences not included in following:
Centric reflections: 82285
Resolution range: 12.7805 0.7083

use_set_completion: False
solvent_radius: 1.20
shrink_truncation_radius: 1.20
van der Waals radii:
   Br     C     H     N    Ni
 1.85  1.70  1.09  1.55  1.63

Total solvent accessible volume / cell = 1162.1 Ang^3 [16.0%]
Total electron count / cell = 106.5

gridding: (128,108,108)
Void #Grid points Vol/A^3 Vol/%  Centre of mass (frac)   Eigenvectors (frac)
   1         2073    10.1   0.1  (-0.016, 0.116, 0.550)  1  ( 0.379,-0.417, 0.826)
                                                         2  (-0.200, 0.835, 0.513)
                                                         3  ( 0.903, 0.360,-0.233)
   2         2073    10.1   0.1  (-0.016, 0.384, 0.050)  1  ( 0.379, 0.417, 0.826)
                                                         2  ( 0.200, 0.835,-0.513)
                                                         3  ( 0.903,-0.360,-0.233)
   3         2073    10.1   0.1  ( 0.016, 0.616, 0.950)  1  ( 0.379, 0.417, 0.826)
                                                         2  ( 0.200, 0.835,-0.513)
                                                         3  ( 0.903,-0.360,-0.233)
   4         2073    10.1   0.1  ( 0.016, 0.884, 0.450)  1  ( 0.379,-0.417, 0.826)
                                                         2  (-0.200, 0.835, 0.513)
                                                         3  ( 0.903, 0.360,-0.233)
   5       111004   540.7   7.4  ( 0.250, 0.750,-0.859)  1  ( 0.965,-0.005, 0.264)
                                                         2  ( 0.005, 1.000, 0.001)
                                                         3  (-0.264, 0.000, 0.965)
   6         2073    10.1   0.1  ( 0.484, 0.616, 0.050)  1  ( 0.379,-0.417, 0.826)
                                                         2  (-0.200, 0.835, 0.513)
                                                         3  ( 0.903, 0.360,-0.233)
   7         2073    10.1   0.1  ( 0.484, 0.884, 0.550)  1  ( 0.379, 0.417, 0.826)
                                                         2  ( 0.200, 0.835,-0.513)
                                                         3  ( 0.903,-0.360,-0.233)
   8         2073    10.1   0.1  ( 0.516, 0.116, 0.450)  1  ( 0.379, 0.417, 0.826)
                                                         2  ( 0.200, 0.835,-0.513)
                                                         3  ( 0.903,-0.360,-0.233)
   9         2073    10.1   0.1  ( 0.516, 0.384, 0.950)  1  ( 0.379,-0.417, 0.826)
                                                         2  (-0.200, 0.835, 0.513)
                                                         3  ( 0.903, 0.360,-0.233)
  10       111004   540.7   7.4  ( 0.750, 0.250,-0.359)  1  ( 0.965,-0.005, 0.264)
                                                         2  ( 0.005, 1.000, 0.001)
                                                         3  (-0.264, 0.000, 0.965)

Void  Vol/Ang^3  #Electrons
   1       10.1          0.0
   2       10.1          0.0
   3       10.1          0.0
   4       10.1          0.0
   5      540.7         53.3
   6       10.1          0.0
   7       10.1          0.0
   8       10.1          0.0
   9       10.1          0.0
  10      540.7         53.3



 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         10702
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0427P)²+10.0313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0963
_refine_special_details          ?
_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
Br1 Br 0.79443(2) 0.64508(2) 0.42598(2) 0.02968(7) Uani 1 1 d . . . . .
Br2 Br 0.81590(2) 0.48951(2) 0.59386(2) 0.02468(6) Uani 1 1 d . . . . .
Ni1 Ni 0.750000 0.56219(2) 0.500000 0.01871(9) Uani 1 2 d S T P . .
N1 N 0.58685(7) 0.74634(10) 0.37626(9) 0.0155(3) Uani 1 1 d . . . . .
N2 N 0.51780(8) 0.66937(10) 0.39742(10) 0.0169(3) Uani 1 1 d . . . . .
C1 C 0.52614(9) 0.73874(11) 0.37370(11) 0.0149(4) Uani 1 1 d . . . . .
C2 C 0.61717(10) 0.68095(12) 0.40226(12) 0.0200(4) Uani 1 1 d . . . . .
H2 H 0.659290 0.671939 0.409447 0.024 Uiso 1 1 calc R . . . .
C3 C 0.57451(10) 0.63271(13) 0.41528(12) 0.0210(4) Uani 1 1 d . . . . .
H3 H 0.581546 0.584076 0.432876 0.025 Uiso 1 1 calc R . . . .
C4 C 0.61760(9) 0.80900(12) 0.35097(11) 0.0166(4) Uani 1 1 d . . . . .
C5 C 0.63262(10) 0.87161(12) 0.39599(12) 0.0202(4) Uani 1 1 d . . . . .
C6 C 0.66726(10) 0.92715(13) 0.37132(13) 0.0244(5) Uani 1 1 d . . . . .
H6 H 0.678442 0.970015 0.399309 0.029 Uiso 1 1 calc R . . . .
C7 C 0.68518(10) 0.91918(13) 0.30561(13) 0.0254(5) Uani 1 1 d . . . . .
H7 H 0.709227 0.956143 0.290999 0.030 Uiso 1 1 calc R . . . .
C8 C 0.66792(10) 0.85732(13) 0.26158(12) 0.0228(5) Uani 1 1 d . . . . .
H8 H 0.679110 0.854044 0.216926 0.027 Uiso 1 1 calc R . . . .
C9 C 0.63388(9) 0.79979(12) 0.28348(12) 0.0187(4) Uani 1 1 d . . . . .
C10 C 0.61486(11) 0.87998(14) 0.46884(12) 0.0260(5) Uani 1 1 d . . . . .
H10 H 0.590616 0.835827 0.475583 0.031 Uiso 1 1 calc R . . . .
C11 C 0.57421(16) 0.94874(17) 0.46938(18) 0.0462(7) Uani 1 1 d . . . . .
H11A H 0.596649 0.992965 0.462280 0.069 Uiso 1 1 calc GR . . . .
H11B H 0.562652 0.951824 0.515488 0.069 Uiso 1 1 calc GR . . . .
H11C H 0.537770 0.944675 0.430705 0.069 Uiso 1 1 calc GR . . . .
C12 C 0.67202(14) 0.8818(2) 0.53187(14) 0.0458(8) Uani 1 1 d . . . . .
H12A H 0.695618 0.836883 0.531183 0.069 Uiso 1 1 calc GR . . . .
H12B H 0.659550 0.885035 0.577422 0.069 Uiso 1 1 calc GR . . . .
H12C H 0.696825 0.924477 0.526617 0.069 Uiso 1 1 calc GR . . . .
C13 C 0.61814(10) 0.72991(13) 0.23649(12) 0.0219(4) Uani 1 1 d . . . . .
H13 H 0.591356 0.698534 0.258853 0.026 Uiso 1 1 calc R . . . .
C14 C 0.58279(10) 0.74817(15) 0.15857(13) 0.0271(5) Uani 1 1 d . . . . .
H14A H 0.545217 0.773848 0.160134 0.041 Uiso 1 1 calc GR . . . .
H14B H 0.573226 0.702594 0.131258 0.041 Uiso 1 1 calc GR . . . .
H14C H 0.607758 0.779523 0.135437 0.041 Uiso 1 1 calc GR . . . .
C15 C 0.67628(11) 0.68447(15) 0.23522(13) 0.0303(5) Uani 1 1 d . . . . .
H15A H 0.701320 0.711592 0.208652 0.045 Uiso 1 1 calc GR . . . .
H15B H 0.664664 0.637191 0.211824 0.045 Uiso 1 1 calc GR . . . .
H15C H 0.699280 0.676167 0.284397 0.045 Uiso 1 1 calc GR . . . .
C16 C 0.45869(9) 0.63233(12) 0.38793(12) 0.0184(4) Uani 1 1 d . . . . .
C17 C 0.43332(10) 0.62053(12) 0.44856(12) 0.0208(4) Uani 1 1 d . . . . .
C18 C 0.37699(11) 0.58200(15) 0.43600(14) 0.0303(5) Uani 1 1 d . . . . .
H18 H 0.358684 0.572712 0.474941 0.036 Uiso 1 1 calc R . . . .
C19 C 0.34817(12) 0.55757(16) 0.36687(15) 0.0366(6) Uani 1 1 d . . . . .
H19 H 0.310813 0.532100 0.359656 0.044 Uiso 1 1 calc R . . . .
C20 C 0.37476(12) 0.57090(16) 0.30843(14) 0.0344(6) Uani 1 1 d . . . . .
H20 H 0.354414 0.555017 0.262035 0.041 Uiso 1 1 calc R . . . .
C21 C 0.43108(11) 0.60741(13) 0.31719(13) 0.0240(5) Uani 1 1 d . . . . .
C22 C 0.46435(10) 0.64665(12) 0.52471(12) 0.0210(4) Uani 1 1 d . . . . .
H22 H 0.497493 0.681505 0.520960 0.025 Uiso 1 1 calc R . . . .
C23 C 0.41876(11) 0.68747(14) 0.56157(13) 0.0273(5) Uani 1 1 d . . . . .
H23A H 0.399809 0.728013 0.531001 0.041 Uiso 1 1 calc GR . . . .
H23B H 0.440481 0.706816 0.608006 0.041 Uiso 1 1 calc GR . . . .
H23C H 0.387518 0.653083 0.568729 0.041 Uiso 1 1 calc GR . . . .
C24 C 0.49292(12) 0.57988(14) 0.57203(14) 0.0305(5) Uani 1 1 d . . . . .
H24A H 0.460910 0.545561 0.576929 0.046 Uiso 1 1 calc GR . . . .
H24B H 0.513895 0.597428 0.619505 0.046 Uiso 1 1 calc GR . . . .
H24C H 0.521810 0.554912 0.549232 0.046 Uiso 1 1 calc GR . . . .
C25 C 0.46144(11) 0.61595(14) 0.25265(13) 0.0269(5) Uani 1 1 d . . . . .
H25 H 0.491994 0.656238 0.264374 0.032 Uiso 1 1 calc R . . . .
C26 C 0.41595(14) 0.63676(16) 0.18164(15) 0.0382(6) Uani 1 1 d . . . . .
H26A H 0.388123 0.595797 0.166101 0.057 Uiso 1 1 calc GR . . . .
H26B H 0.438171 0.647372 0.144615 0.057 Uiso 1 1 calc GR . . . .
H26C H 0.392925 0.680217 0.189507 0.057 Uiso 1 1 calc GR . . . .
C27 C 0.49567(15) 0.54405(18) 0.24231(16) 0.0419(7) Uani 1 1 d . . . . .
H27A H 0.525371 0.532583 0.286663 0.063 Uiso 1 1 calc GR . . . .
H27B H 0.516466 0.550765 0.203280 0.063 Uiso 1 1 calc GR . . . .
H27C H 0.466669 0.503627 0.230500 0.063 Uiso 1 1 calc GR . . . .
C28 C 0.47758(9) 0.79512(11) 0.35289(11) 0.0160(4) Uani 1 1 d . . . . .
C29 C 0.44139(10) 0.81238(13) 0.40234(12) 0.0233(5) Uani 1 1 d . . . . .
H29 H 0.449084 0.789020 0.447757 0.028 Uiso 1 1 calc R . . . .
C30 C 0.39427(11) 0.86393(14) 0.38407(13) 0.0277(5) Uani 1 1 d . . . . .
H30 H 0.370920 0.875414 0.417817 0.033 Uiso 1 1 calc R . . . .
C31 C 0.38092(11) 0.89912(14) 0.31625(13) 0.0259(5) Uani 1 1 d . . . . .
C32 C 0.41743(11) 0.88168(14) 0.26739(13) 0.0254(5) Uani 1 1 d . . . . .
H32 H 0.409405 0.904758 0.221824 0.031 Uiso 1 1 calc R . . . .
C33 C 0.46550(10) 0.83065(13) 0.28523(12) 0.0213(4) Uani 1 1 d . . . . .
H33 H 0.489603 0.820199 0.252021 0.026 Uiso 1 1 calc R . . . .
C34 C 0.32774(14) 0.95348(17) 0.29590(16) 0.0428(7) Uani 1 1 d . . . . .
H34A H 0.336328 0.989228 0.261379 0.064 Uiso 1 1 calc GR . . . .
H34B H 0.322449 0.979138 0.338943 0.064 Uiso 1 1 calc GR . . . .
H34C H 0.290662 0.926622 0.274439 0.064 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
Br1 Ni1 2.3944(3) . ?
Br2 Ni1 2.4010(3) . ?
Ni1 Br1 2.3944(3) 2_656 ?
Ni1 Br2 2.4010(3) 2_656 ?
N1 C1 1.348(2) . ?
N1 C2 1.381(3) . ?
N1 C4 1.447(3) . ?
N2 C1 1.344(3) . ?
N2 C3 1.393(3) . ?
N2 C16 1.447(3) . ?
C1 C28 1.463(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.345(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(3) . ?
C4 C9 1.406(3) . ?
C5 C6 1.399(3) . ?
C5 C10 1.517(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.389(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.381(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.394(3) . ?
C9 C13 1.523(3) . ?
C10 H10 0.9800 . ?
C10 C11 1.527(4) . ?
C10 C12 1.527(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.531(3) . ?
C13 C15 1.532(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.398(3) . ?
C16 C21 1.403(3) . ?
C17 C18 1.402(3) . ?
C17 C22 1.513(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.381(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.382(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.389(3) . ?
C21 C25 1.525(3) . ?
C22 H22 0.9800 . ?
C22 C23 1.537(3) . ?
C22 C24 1.536(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.525(4) . ?
C25 C27 1.528(4) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.396(3) . ?
C28 C33 1.391(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.379(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.391(3) . ?
C31 C32 1.393(3) . ?
C31 C34 1.511(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.387(3) . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 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
Br1 Ni1 Br1 103.60(2) . 2_656 ?
Br1 Ni1 Br2 99.886(8) 2_656 . ?
Br1 Ni1 Br2 119.812(8) . . ?
Br1 Ni1 Br2 119.809(8) 2_656 2_656 ?
Br1 Ni1 Br2 99.888(8) . 2_656 ?
Br2 Ni1 Br2 114.53(2) 2_656 . ?
C1 N1 C2 109.39(17) . . ?
C1 N1 C4 127.69(17) . . ?
C2 N1 C4 122.74(16) . . ?
C1 N2 C3 109.10(17) . . ?
C1 N2 C16 124.85(17) . . ?
C3 N2 C16 124.25(18) . . ?
N1 C1 C28 127.82(18) . . ?
N2 C1 N1 107.12(17) . . ?
N2 C1 C28 125.00(18) . . ?
N1 C2 H2 126.3 . . ?
C3 C2 N1 107.35(18) . . ?
C3 C2 H2 126.3 . . ?
N2 C3 H3 126.5 . . ?
C2 C3 N2 107.04(19) . . ?
C2 C3 H3 126.5 . . ?
C5 C4 N1 119.10(18) . . ?
C5 C4 C9 124.39(19) . . ?
C9 C4 N1 116.38(19) . . ?
C4 C5 C6 116.2(2) . . ?
C4 C5 C10 123.37(19) . . ?
C6 C5 C10 120.4(2) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 120.9(2) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.2(2) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.6(2) . . ?
C9 C8 H8 119.7 . . ?
C4 C9 C13 123.12(19) . . ?
C8 C9 C4 116.7(2) . . ?
C8 C9 C13 120.12(19) . . ?
C5 C10 H10 107.6 . . ?
C5 C10 C11 111.2(2) . . ?
C5 C10 C12 111.1(2) . . ?
C11 C10 H10 107.6 . . ?
C11 C10 C12 111.6(2) . . ?
C12 C10 H10 107.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 107.6 . . ?
C9 C13 C14 112.32(19) . . ?
C9 C13 C15 111.11(18) . . ?
C14 C13 H13 107.6 . . ?
C14 C13 C15 110.44(19) . . ?
C15 C13 H13 107.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 119.58(19) . . ?
C17 C16 C21 123.58(19) . . ?
C21 C16 N2 116.79(19) . . ?
C16 C17 C18 116.7(2) . . ?
C16 C17 C22 122.82(19) . . ?
C18 C17 C22 120.5(2) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 C17 121.2(2) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.1(2) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.2 . . ?
C19 C20 C21 121.7(2) . . ?
C21 C20 H20 119.2 . . ?
C16 C21 C25 123.0(2) . . ?
C20 C21 C16 116.7(2) . . ?
C20 C21 C25 120.3(2) . . ?
C17 C22 H22 108.4 . . ?
C17 C22 C23 111.52(19) . . ?
C17 C22 C24 110.30(19) . . ?
C23 C22 H22 108.4 . . ?
C24 C22 H22 108.4 . . ?
C24 C22 C23 109.64(19) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.8 . . ?
C21 C25 C26 113.2(2) . . ?
C21 C25 C27 110.0(2) . . ?
C26 C25 H25 107.8 . . ?
C26 C25 C27 110.1(2) . . ?
C27 C25 H25 107.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 118.51(19) . . ?
C33 C28 C1 122.33(19) . . ?
C33 C28 C29 119.14(19) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.2(2) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.3 . . ?
C29 C30 C31 121.4(2) . . ?
C31 C30 H30 119.3 . . ?
C30 C31 C32 117.9(2) . . ?
C30 C31 C34 120.9(2) . . ?
C32 C31 C34 121.2(2) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.4(2) . . ?
C33 C32 H32 119.3 . . ?
C28 C33 H33 120.1 . . ?
C32 C33 C28 119.9(2) . . ?
C32 C33 H33 120.1 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C28 C29 -123.9(2) . . . . ?
N1 C1 C28 C33 57.5(3) . . . . ?
N1 C2 C3 N2 -0.4(2) . . . . ?
N1 C4 C5 C6 174.29(18) . . . . ?
N1 C4 C5 C10 -4.0(3) . . . . ?
N1 C4 C9 C8 -174.92(17) . . . . ?
N1 C4 C9 C13 2.7(3) . . . . ?
N2 C1 C28 C29 52.8(3) . . . . ?
N2 C1 C28 C33 -125.8(2) . . . . ?
N2 C16 C17 C18 -177.8(2) . . . . ?
N2 C16 C17 C22 1.5(3) . . . . ?
N2 C16 C21 C20 179.1(2) . . . . ?
N2 C16 C21 C25 1.8(3) . . . . ?
C1 N1 C2 C3 0.4(2) . . . . ?
C1 N1 C4 C5 82.1(3) . . . . ?
C1 N1 C4 C9 -102.0(2) . . . . ?
C1 N2 C3 C2 0.2(2) . . . . ?
C1 N2 C16 C17 -109.6(2) . . . . ?
C1 N2 C16 C21 72.9(3) . . . . ?
C1 C28 C29 C30 -178.5(2) . . . . ?
C1 C28 C33 C32 177.7(2) . . . . ?
C2 N1 C1 N2 -0.3(2) . . . . ?
C2 N1 C1 C28 176.9(2) . . . . ?
C2 N1 C4 C5 -103.4(2) . . . . ?
C2 N1 C4 C9 72.6(2) . . . . ?
C3 N2 C1 N1 0.0(2) . . . . ?
C3 N2 C1 C28 -177.26(19) . . . . ?
C3 N2 C16 C17 87.4(3) . . . . ?
C3 N2 C16 C21 -90.1(3) . . . . ?
C4 N1 C1 N2 174.87(19) . . . . ?
C4 N1 C1 C28 -7.9(3) . . . . ?
C4 N1 C2 C3 -175.03(19) . . . . ?
C4 C5 C6 C7 0.0(3) . . . . ?
C4 C5 C10 C11 -120.0(2) . . . . ?
C4 C5 C10 C12 115.1(3) . . . . ?
C4 C9 C13 C14 125.4(2) . . . . ?
C4 C9 C13 C15 -110.4(2) . . . . ?
C5 C4 C9 C8 0.8(3) . . . . ?
C5 C4 C9 C13 178.45(19) . . . . ?
C5 C6 C7 C8 1.9(3) . . . . ?
C6 C5 C10 C11 61.8(3) . . . . ?
C6 C5 C10 C12 -63.1(3) . . . . ?
C6 C7 C8 C9 -2.4(3) . . . . ?
C7 C8 C9 C4 1.1(3) . . . . ?
C7 C8 C9 C13 -176.62(19) . . . . ?
C8 C9 C13 C14 -57.1(3) . . . . ?
C8 C9 C13 C15 67.2(3) . . . . ?
C9 C4 C5 C6 -1.3(3) . . . . ?
C9 C4 C5 C10 -179.6(2) . . . . ?
C10 C5 C6 C7 178.3(2) . . . . ?
C16 N2 C1 N1 -165.17(18) . . . . ?
C16 N2 C1 C28 17.5(3) . . . . ?
C16 N2 C3 C2 165.5(2) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
C16 C17 C22 C23 132.5(2) . . . . ?
C16 C17 C22 C24 -105.4(2) . . . . ?
C16 C21 C25 C26 -140.7(2) . . . . ?
C16 C21 C25 C27 95.7(3) . . . . ?
C17 C16 C21 C20 1.7(4) . . . . ?
C17 C16 C21 C25 -175.7(2) . . . . ?
C17 C18 C19 C20 0.0(4) . . . . ?
C18 C17 C22 C23 -48.2(3) . . . . ?
C18 C17 C22 C24 73.9(3) . . . . ?
C18 C19 C20 C21 1.3(5) . . . . ?
C19 C20 C21 C16 -2.1(4) . . . . ?
C19 C20 C21 C25 175.3(3) . . . . ?
C20 C21 C25 C26 42.1(3) . . . . ?
C20 C21 C25 C27 -81.5(3) . . . . ?
C21 C16 C17 C18 -0.5(3) . . . . ?
C21 C16 C17 C22 178.9(2) . . . . ?
C22 C17 C18 C19 -179.8(2) . . . . ?
C28 C29 C30 C31 0.9(4) . . . . ?
C29 C28 C33 C32 -0.9(3) . . . . ?
C29 C30 C31 C32 -1.1(4) . . . . ?
C29 C30 C31 C34 177.8(3) . . . . ?
C30 C31 C32 C33 0.3(4) . . . . ?
C31 C32 C33 C28 0.7(4) . . . . ?
C33 C28 C29 C30 0.1(3) . . . . ?
C34 C31 C32 C33 -178.6(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.016 0.116 0.550 10.1 0.0 ?
2 -0.016 0.384 0.050 10.1 0.0 ?
3 0.016 0.616 0.950 10.1 0.0 ?
4 0.016 0.884 0.450 10.1 0.0 ?
5 0.250 0.750 -0.859 540.7 53.3 ?
6 0.484 0.616 0.050 10.1 0.0 ?
7 0.484 0.884 0.550 10.1 0.0 ?
8 0.516 0.116 0.450 10.1 0.0 ?
9 0.516 0.384 0.950 10.1 0.0 ?
10 0.750 0.250 -0.359 540.7 53.3 ?

_olex2_date_sample_data_collection 2017-01-31
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.824

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
####################################################################### 
# 
# 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_compound_26
_database_code_depnum_ccdc_archive 'CCDC 1559111'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;


_audit_creation_date             2017-06-21
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H45 Br Cu N3, 2(C7 H8)'
_chemical_formula_sum            'C49 H61 Br Cu N3'
_chemical_formula_weight         835.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C51 H60 N3 Cu Br'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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      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                   12.2492(2)
_cell_length_b                   12.9626(2)
_cell_length_c                   15.7524(3)
_cell_angle_alpha                82.7553(15)
_cell_angle_beta                 77.8500(15)
_cell_angle_gamma                65.2414(18)
_cell_volume                     2218.39(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    31311
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      31.1810
_cell_measurement_theta_min      1.8320
_exptl_absorpt_coefficient_mu    1.428
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             880
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0543
-5 5 2 0.1122
5 -5 -2 0.1122
0 0 -1 0.0543
5 4 4 0.1742
-1 -5 -4 0.1543
1 5 4 0.1543
-5 -4 -4 0.1742
-1 -1 5 0.0592

_exptl_crystal_size_max          0.433
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.109
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0017 0.0003 0.9968 0.0074 0.0388 -0.0236
-4.9959 4.9974 1.9881 -0.4683 0.1011 -0.2476
4.9959 -4.9974 -1.9881 0.4683 -0.1011 0.2476
0.0017 -0.0003 -0.9968 -0.0074 -0.0388 0.0236
4.9945 3.9938 3.9916 0.1761 -0.0609 -0.2723
-0.9976 -4.9948 -3.9876 0.0982 -0.0221 0.3065
0.9976 4.9948 3.9876 -0.0982 0.0221 -0.3065
-4.9945 -3.9938 -3.9916 -0.1761 0.0609 0.2723
-0.9953 -1.0024 5.0040 0.0165 0.2419 -0.0741

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            100993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         1.732
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  96.00   1.00   15.00    --   25.96  77.00  30.00  100
  2  ω      6.00  95.00   1.00   15.00    --   25.96  57.00-180.00   89
  3  ω    -43.00  47.00   1.00   15.00    --   25.96 -57.00 -90.00   90
  4  ω    -44.00  56.00   1.00   15.00    --   25.96 -77.00-180.00  100
  5  ω    -20.00  68.00   1.00   15.00    --   25.96 -99.00-120.00   88
  6  ω     -4.00  96.00   1.00   15.00    --   25.96  77.00 -60.00  100
  7  ω      0.00  98.00   1.00   15.00    --   25.96  38.00 150.00   98
  8  ω    -44.00  56.00   1.00   15.00    --   25.96 -77.00  90.00  100
  9  ω     -4.00  96.00   1.00   15.00    --   25.96  77.00-150.00  100
 10  ω    -20.00  68.00   1.00   15.00    --   25.96 -99.00  30.00   88
 11  ω    -99.00 -35.00   1.00   15.00    --  -23.50-178.00 120.00   64
 12  ω     35.00 102.00   1.00   15.00    --   25.96 178.00  90.00   67
 13  ω      6.00  95.00   1.00   15.00    --   25.96  57.00  30.00   89
 14  ω    -20.00  68.00   1.00   15.00    --   25.96 -99.00-180.00   88
 15  ω    -46.00  51.00   1.00   15.00    --   25.96 -38.00  90.00   97
 16  ω    -47.00  99.00   1.00   15.00    --   25.96   0.00-180.00  146
 17  ω    -47.00  99.00   1.00   15.00    --   25.96   0.00-150.00  146
 18  ω    -47.00  99.00   1.00   15.00    --   25.96   0.00-120.00  146
 19  ω    -47.00  66.00   1.00   15.00    --   25.96   0.00 -90.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0592196000
_diffrn_orient_matrix_UB_12      -0.0375146000
_diffrn_orient_matrix_UB_13      0.0075531000
_diffrn_orient_matrix_UB_21      -0.0261517000
_diffrn_orient_matrix_UB_22      -0.0213742000
_diffrn_orient_matrix_UB_23      0.0388593000
_diffrn_orient_matrix_UB_31      -0.0019628000
_diffrn_orient_matrix_UB_32      -0.0421123000
_diffrn_orient_matrix_UB_33      -0.0236281000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10831
_reflns_number_total             13038
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_reflns_special_details          
;
 Disorder of two toluene over two sites near inversion center. They were 
 constrained with EADP to have the same displacement parameters. 
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.030
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         13038
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0495
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0607P)²+3.7449P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1403
_refine_special_details          ?
_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
Br1 Br 0.31667(3) 0.93376(2) -0.19994(2) 0.03208(8) Uani 1 1 d . . . . .
Cu1 Cu 0.28322(3) 0.87325(2) -0.06096(2) 0.02280(8) Uani 1 1 d . . . . .
N1 N 0.22983(17) 0.69302(15) 0.16599(12) 0.0188(3) Uani 1 1 d . . . . .
N2 N 0.25374(17) 0.84977(15) 0.13105(12) 0.0188(3) Uani 1 1 d . . . . .
N3 N 0.2615(2) 0.8384(2) 0.54403(14) 0.0291(4) Uani 1 1 d . . . . .
C1 C 0.2388(2) 0.77954(18) 0.19898(14) 0.0187(4) Uani 1 1 d . . . . .
C2 C 0.2391(2) 0.71095(19) 0.07668(15) 0.0211(4) Uani 1 1 d . . . . .
H2 H 0.234830 0.663212 0.039260 0.025 Uiso 1 1 calc R . . . .
C3 C 0.2554(2) 0.80942(19) 0.05161(15) 0.0208(4) Uani 1 1 d . . . . .
C4 C 0.2052(2) 0.60042(18) 0.21378(15) 0.0196(4) Uani 1 1 d . . . . .
C5 C 0.3033(2) 0.49403(19) 0.21717(15) 0.0218(4) Uani 1 1 d . . . . .
C6 C 0.2765(3) 0.4049(2) 0.26171(17) 0.0277(5) Uani 1 1 d . . . . .
H6 H 0.339205 0.333376 0.266139 0.033 Uiso 1 1 calc R . . . .
C7 C 0.1578(3) 0.4218(2) 0.29937(18) 0.0328(6) Uani 1 1 d . . . . .
H7 H 0.141590 0.361347 0.328523 0.039 Uiso 1 1 calc R . . . .
C8 C 0.0629(3) 0.5278(2) 0.29404(18) 0.0318(5) Uani 1 1 d . . . . .
H8 H -0.016276 0.537481 0.319732 0.038 Uiso 1 1 calc R . . . .
C9 C 0.0841(2) 0.62024(19) 0.25075(16) 0.0235(4) Uani 1 1 d . . . . .
C10 C 0.4322(2) 0.4728(2) 0.1720(2) 0.0323(6) Uani 1 1 d . . . . .
H10 H 0.436391 0.546484 0.154531 0.039 Uiso 1 1 calc R . . . .
C11 C 0.5269(3) 0.4078(3) 0.2311(3) 0.0505(9) Uani 1 1 d . . . . .
H11A H 0.505889 0.448393 0.283088 0.076 Uiso 1 1 calc GR . . . .
H11B H 0.606272 0.400886 0.201085 0.076 Uiso 1 1 calc GR . . . .
H11C H 0.527645 0.333352 0.245994 0.076 Uiso 1 1 calc GR . . . .
C12 C 0.4626(3) 0.4072(3) 0.0900(2) 0.0426(7) Uani 1 1 d . . . . .
H12A H 0.461952 0.333472 0.105990 0.064 Uiso 1 1 calc GR . . . .
H12B H 0.542042 0.398763 0.059063 0.064 Uiso 1 1 calc GR . . . .
H12C H 0.402858 0.448213 0.053590 0.064 Uiso 1 1 calc GR . . . .
C13 C -0.0214(2) 0.7346(2) 0.24286(19) 0.0291(5) Uani 1 1 d . . . . .
H13 H 0.012566 0.788064 0.212048 0.035 Uiso 1 1 calc R . . . .
C14 C -0.0890(4) 0.7805(3) 0.3314(3) 0.0590(10) Uani 1 1 d . . . . .
H14A H -0.120249 0.728008 0.363961 0.089 Uiso 1 1 calc GR . . . .
H14B H -0.155451 0.852539 0.324331 0.089 Uiso 1 1 calc GR . . . .
H14C H -0.034080 0.790219 0.361926 0.089 Uiso 1 1 calc GR . . . .
C15 C -0.1073(3) 0.7266(3) 0.1890(3) 0.0458(8) Uani 1 1 d . . . . .
H15A H -0.061563 0.694733 0.134265 0.069 Uiso 1 1 calc GR . . . .
H15B H -0.168144 0.801219 0.179138 0.069 Uiso 1 1 calc GR . . . .
H15C H -0.146421 0.678894 0.219804 0.069 Uiso 1 1 calc GR . . . .
C16 C 0.2777(2) 0.94795(19) 0.13855(15) 0.0199(4) Uani 1 1 d . . . . .
C17 C 0.1824(2) 1.05606(19) 0.13665(16) 0.0236(4) Uani 1 1 d . . . . .
C18 C 0.2079(3) 1.1485(2) 0.14730(19) 0.0312(5) Uani 1 1 d . . . . .
H18 H 0.146992 1.221632 0.146274 0.037 Uiso 1 1 calc R . . . .
C19 C 0.3223(3) 1.1329(3) 0.15934(19) 0.0353(6) Uani 1 1 d . . . . .
H19 H 0.337170 1.195452 0.167382 0.042 Uiso 1 1 calc R . . . .
C20 C 0.4145(3) 1.0258(3) 0.15955(19) 0.0333(6) Uani 1 1 d . . . . .
H20 H 0.491278 1.017025 0.167011 0.040 Uiso 1 1 calc R . . . .
C21 C 0.3951(2) 0.9299(2) 0.14878(16) 0.0248(5) Uani 1 1 d . . . . .
C22 C 0.0568(2) 1.0757(2) 0.1214(2) 0.0324(6) Uani 1 1 d . . . . .
H22 H 0.050495 1.002205 0.127172 0.039 Uiso 1 1 calc R . . . .
C23 C -0.0454(3) 1.1548(3) 0.1881(2) 0.0415(7) Uani 1 1 d . . . . .
H23A H -0.032464 1.124885 0.245748 0.062 Uiso 1 1 calc GR . . . .
H23B H -0.122861 1.159708 0.179768 0.062 Uiso 1 1 calc GR . . . .
H23C H -0.044596 1.229161 0.180272 0.062 Uiso 1 1 calc GR . . . .
C24 C 0.0413(3) 1.1248(3) 0.0297(2) 0.0441(7) Uani 1 1 d . . . . .
H24A H 0.041232 1.199467 0.024089 0.066 Uiso 1 1 calc GR . . . .
H24B H -0.034705 1.129532 0.018345 0.066 Uiso 1 1 calc GR . . . .
H24C H 0.107424 1.076550 -0.011249 0.066 Uiso 1 1 calc GR . . . .
C25 C 0.4995(2) 0.8142(2) 0.1455(2) 0.0341(6) Uani 1 1 d . . . . .
H25 H 0.467096 0.757301 0.143159 0.041 Uiso 1 1 calc R . . . .
C26 C 0.5590(3) 0.7867(3) 0.2269(3) 0.0524(9) Uani 1 1 d . . . . .
H26A H 0.594748 0.839410 0.228893 0.079 Uiso 1 1 calc GR . . . .
H26B H 0.621345 0.710705 0.224665 0.079 Uiso 1 1 calc GR . . . .
H26C H 0.498185 0.792737 0.277854 0.079 Uiso 1 1 calc GR . . . .
C27 C 0.5936(3) 0.8079(3) 0.0625(3) 0.0550(9) Uani 1 1 d . . . . .
H27A H 0.555597 0.820205 0.012528 0.083 Uiso 1 1 calc GR . . . .
H27B H 0.660130 0.734333 0.060737 0.083 Uiso 1 1 calc GR . . . .
H27C H 0.623790 0.865394 0.062321 0.083 Uiso 1 1 calc GR . . . .
C28 C 0.2390(2) 0.79263(19) 0.28953(15) 0.0197(4) Uani 1 1 d . . . . .
C29 C 0.1721(2) 0.89697(19) 0.32806(15) 0.0230(4) Uani 1 1 d . . . . .
H29 H 0.121542 0.957541 0.296851 0.028 Uiso 1 1 calc R . . . .
C30 C 0.1790(2) 0.9126(2) 0.41172(15) 0.0245(4) Uani 1 1 d . . . . .
H30 H 0.132995 0.983198 0.435778 0.029 Uiso 1 1 calc R . . . .
C31 C 0.2551(2) 0.8228(2) 0.46117(15) 0.0235(4) Uani 1 1 d . . . . .
C32 C 0.3205(2) 0.7173(2) 0.42243(16) 0.0263(5) Uani 1 1 d . . . . .
H32 H 0.370446 0.656113 0.453505 0.032 Uiso 1 1 calc R . . . .
C33 C 0.3121(2) 0.7028(2) 0.33927(16) 0.0239(4) Uani 1 1 d . . . . .
H33 H 0.355992 0.631657 0.315575 0.029 Uiso 1 1 calc R . . . .
C34 C 0.1997(3) 0.9509(2) 0.57852(17) 0.0333(6) Uani 1 1 d . . . . .
H34A H 0.235284 1.000124 0.545542 0.050 Uiso 1 1 calc GR . . . .
H34B H 0.208129 0.946583 0.638234 0.050 Uiso 1 1 calc GR . . . .
H34C H 0.114663 0.980526 0.574638 0.050 Uiso 1 1 calc GR . . . .
C35 C 0.3620(3) 0.7574(3) 0.58477(19) 0.0369(6) Uani 1 1 d . . . . .
H35A H 0.361222 0.683238 0.587897 0.055 Uiso 1 1 calc GR . . . .
H35B H 0.353289 0.780145 0.642350 0.055 Uiso 1 1 calc GR . . . .
H35C H 0.437857 0.755243 0.550999 0.055 Uiso 1 1 calc GR . . . .
C36 C 0.8985(3) 0.3583(3) 0.4254(2) 0.0396(7) Uani 1 1 d D . . . .
C37 C 0.8328(3) 0.3917(3) 0.3579(2) 0.0476(5) Uani 1 1 d D . . . .
H37 H 0.853650 0.342041 0.313663 0.057 Uiso 1 1 calc R . . . .
C38 C 0.7368(4) 0.4973(3) 0.3548(3) 0.0536(5) Uani 1 1 d D . . . .
H38 H 0.694462 0.517914 0.308544 0.064 Uiso 1 1 calc R . . . .
C39 C 0.7039(4) 0.5717(3) 0.4196(3) 0.0541(8) Uani 1 1 d D . . . .
H39 H 0.638596 0.642149 0.418246 0.065 Uiso 1 1 calc R . . . .
C40 C 0.7688(4) 0.5405(3) 0.4860(3) 0.0536(5) Uani 1 1 d D . . . .
H40 H 0.748254 0.590883 0.529572 0.064 Uiso 1 1 calc R . . . .
C41 C 0.8648(3) 0.4346(3) 0.4894(2) 0.0476(5) Uani 1 1 d D . . . .
H41 H 0.907148 0.414801 0.535643 0.057 Uiso 1 1 calc R . . . .
C42 C 1.0000(3) 0.2421(3) 0.4298(3) 0.0564(8) Uani 1 1 d D . . . .
H42A H 0.968457 0.191150 0.464815 0.085 Uiso 1 1 calc GR . . . .
H42B H 1.062557 0.246488 0.455173 0.085 Uiso 1 1 calc GR . . . .
H42C H 1.033726 0.214462 0.372238 0.085 Uiso 1 1 calc GR . . . .
C43 C 0.8988(11) 0.4925(12) 0.0381(6) 0.051(2) Uani 0.5 1 d D . P A -1
C44 C 1.0024(8) 0.4628(9) 0.0816(6) 0.0476(5) Uani 0.5 1 d D . P A -1
H44 H 0.997912 0.436567 0.139475 0.057 Uiso 0.5 1 calc R . P A -1
C45 C 1.1064(9) 0.4732(10) 0.0376(7) 0.0536(5) Uani 0.5 1 d D . P A -1
H45 H 1.172246 0.455070 0.065579 0.064 Uiso 0.5 1 calc R . P A -1
C46 C 1.1130(12) 0.5113(15) -0.0493(9) 0.0541(8) Uani 0.5 1 d D . P A -1
H46 H 1.184119 0.518291 -0.078422 0.065 Uiso 0.5 1 calc R . P A -1
C47 C 1.0229(8) 0.5375(10) -0.0917(7) 0.0536(5) Uani 0.5 1 d D . P A -1
H47 H 1.031330 0.561122 -0.150037 0.064 Uiso 0.5 1 calc R . P A -1
C48 C 0.9157(9) 0.5300(9) -0.0497(6) 0.0476(5) Uani 0.5 1 d D . P A -1
H48 H 0.852039 0.550466 -0.080390 0.057 Uiso 0.5 1 calc R . P A -1
C49 C 0.7895(6) 0.4773(6) 0.0906(6) 0.0564(8) Uani 0.5 1 d D . P A -1
H49A H 0.807718 0.397657 0.100497 0.085 Uiso 0.5 1 calc GR . P A -1
H49B H 0.722284 0.512266 0.059595 0.085 Uiso 0.5 1 calc GR . P A -1
H49C H 0.768145 0.512270 0.145301 0.085 Uiso 0.5 1 calc GR . P A -1
C50 C 0.5283(6) 0.9690(6) 0.5329(4) 0.0478(16) Uani 0.5 1 d D . P B -1
C51 C 0.5440(9) 0.9426(7) 0.4423(5) 0.0476(5) Uani 0.5 1 d D . P B -1
H51 H 0.612058 0.879357 0.420181 0.057 Uiso 0.5 1 calc R . P B -1
C52 C 0.4695(7) 1.0016(6) 0.3928(5) 0.0536(5) Uani 0.5 1 d D . P B -1
H52 H 0.473037 0.970886 0.341488 0.064 Uiso 0.5 1 calc R . P B -1
C53 C 0.3778(8) 1.1162(6) 0.4127(6) 0.0541(8) Uani 0.5 1 d D . P B -1
H53 H 0.334310 1.165551 0.371683 0.065 Uiso 0.5 1 calc R . P B -1
C54 C 0.3627(7) 1.1422(6) 0.4893(5) 0.0536(5) Uani 0.5 1 d D . P B -1
H54 H 0.294819 1.207008 0.509028 0.064 Uiso 0.5 1 calc R . P B -1
C55 C 0.4390(9) 1.0819(6) 0.5450(6) 0.0476(5) Uani 0.5 1 d D . P B -1
H55 H 0.432685 1.116667 0.595048 0.057 Uiso 0.5 1 calc R . P B -1
C56 C 0.5985(8) 0.9188(7) 0.5993(6) 0.0564(8) Uani 0.5 1 d D . P B -1
H56A H 0.659631 0.845307 0.582391 0.085 Uiso 0.5 1 calc GR . P B -1
H56B H 0.546282 0.910675 0.652051 0.085 Uiso 0.5 1 calc GR . P B -1
H56C H 0.637250 0.966262 0.608492 0.085 Uiso 0.5 1 calc GR . P B -1


_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
Br1 Cu1 2.2438(4) . ?
Cu1 C3 1.886(2) . ?
N1 C1 1.347(3) . ?
N1 C2 1.385(3) . ?
N1 C4 1.441(3) . ?
N2 C1 1.348(3) . ?
N2 C3 1.409(3) . ?
N2 C16 1.444(3) . ?
N3 C31 1.368(3) . ?
N3 C34 1.448(4) . ?
N3 C35 1.452(4) . ?
C1 C28 1.458(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.371(3) . ?
C4 C5 1.403(3) . ?
C4 C9 1.401(3) . ?
C5 C6 1.396(3) . ?
C5 C10 1.513(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.386(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.396(3) . ?
C9 C13 1.516(3) . ?
C10 H10 0.9800 . ?
C10 C11 1.536(4) . ?
C10 C12 1.529(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13 0.9800 . ?
C13 C14 1.515(4) . ?
C13 C15 1.526(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.400(3) . ?
C16 C21 1.397(3) . ?
C17 C18 1.396(3) . ?
C17 C22 1.517(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.380(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.375(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.396(4) . ?
C21 C25 1.507(4) . ?
C22 H22 0.9800 . ?
C22 C23 1.538(4) . ?
C22 C24 1.520(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25 0.9800 . ?
C25 C26 1.537(4) . ?
C25 C27 1.536(5) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.392(3) . ?
C28 C33 1.402(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.384(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.413(3) . ?
C31 C32 1.404(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.378(3) . ?
C33 H33 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.385(5) . ?
C36 C41 1.378(5) . ?
C36 C42 1.504(4) . ?
C37 H37 0.9300 . ?
C37 C38 1.385(5) . ?
C38 H38 0.9300 . ?
C38 C39 1.373(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.365(5) . ?
C40 H40 0.9300 . ?
C40 C41 1.388(5) . ?
C41 H41 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.455(12) . ?
C43 C48 1.409(10) . ?
C43 C49 1.493(11) . ?
C44 H44 0.9300 . ?
C44 C45 1.367(10) . ?
C45 H45 0.9300 . ?
C45 C46 1.394(12) . ?
C46 H46 0.9300 . ?
C46 C47 1.311(12) . ?
C47 H47 0.9300 . ?
C47 C48 1.377(10) . ?
C48 H48 0.9300 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.465(10) . ?
C50 C55 1.420(10) . ?
C50 C56 1.412(10) . ?
C51 H51 0.9300 . ?
C51 C52 1.260(9) . ?
C52 H52 0.9300 . ?
C52 C53 1.462(9) . ?
C53 H53 0.9300 . ?
C53 C54 1.250(10) . ?
C54 H54 0.9300 . ?
C54 C55 1.348(9) . ?
C55 H55 0.9300 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 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
C3 Cu1 Br1 174.31(7) . . ?
C1 N1 C2 108.70(18) . . ?
C1 N1 C4 127.16(19) . . ?
C2 N1 C4 123.99(18) . . ?
C1 N2 C3 111.89(18) . . ?
C1 N2 C16 123.52(19) . . ?
C3 N2 C16 124.29(18) . . ?
C31 N3 C34 119.7(2) . . ?
C31 N3 C35 119.7(2) . . ?
C34 N3 C35 116.7(2) . . ?
N1 C1 N2 106.51(19) . . ?
N1 C1 C28 127.2(2) . . ?
N2 C1 C28 126.2(2) . . ?
N1 C2 H2 125.0 . . ?
C3 C2 N1 109.97(19) . . ?
C3 C2 H2 125.0 . . ?
N2 C3 Cu1 127.41(16) . . ?
C2 C3 Cu1 129.57(18) . . ?
C2 C3 N2 102.92(19) . . ?
C5 C4 N1 118.1(2) . . ?
C9 C4 N1 118.22(19) . . ?
C9 C4 C5 123.6(2) . . ?
C4 C5 C10 122.7(2) . . ?
C6 C5 C4 117.0(2) . . ?
C6 C5 C10 120.2(2) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.8(2) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.7(2) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 121.1(2) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C13 122.8(2) . . ?
C8 C9 C4 116.8(2) . . ?
C8 C9 C13 120.4(2) . . ?
C5 C10 H10 108.2 . . ?
C5 C10 C11 112.5(3) . . ?
C5 C10 C12 109.5(2) . . ?
C11 C10 H10 108.2 . . ?
C12 C10 H10 108.2 . . ?
C12 C10 C11 110.0(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 107.8 . . ?
C9 C13 C15 110.7(2) . . ?
C14 C13 C9 111.4(3) . . ?
C14 C13 H13 107.8 . . ?
C14 C13 C15 111.4(3) . . ?
C15 C13 H13 107.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N2 118.75(19) . . ?
C21 C16 N2 118.0(2) . . ?
C21 C16 C17 123.2(2) . . ?
C16 C17 C22 123.0(2) . . ?
C18 C17 C16 117.1(2) . . ?
C18 C17 C22 119.9(2) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.0(3) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.6(2) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.3(2) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 C25 123.2(2) . . ?
C20 C21 C16 116.9(2) . . ?
C20 C21 C25 119.9(2) . . ?
C17 C22 H22 108.3 . . ?
C17 C22 C23 111.8(2) . . ?
C17 C22 C24 109.9(2) . . ?
C23 C22 H22 108.3 . . ?
C24 C22 H22 108.3 . . ?
C24 C22 C23 110.2(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 108.2 . . ?
C21 C25 C26 111.5(3) . . ?
C21 C25 C27 109.7(2) . . ?
C26 C25 H25 108.2 . . ?
C27 C25 H25 108.2 . . ?
C27 C25 C26 111.0(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 121.0(2) . . ?
C29 C28 C33 117.6(2) . . ?
C33 C28 C1 121.3(2) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 C28 121.5(2) . . ?
C30 C29 H29 119.3 . . ?
C29 C30 H30 119.5 . . ?
C29 C30 C31 121.0(2) . . ?
C31 C30 H30 119.5 . . ?
N3 C31 C30 120.9(2) . . ?
N3 C31 C32 121.9(2) . . ?
C32 C31 C30 117.1(2) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 C31 121.2(2) . . ?
C33 C32 H32 119.4 . . ?
C28 C33 H33 119.2 . . ?
C32 C33 C28 121.5(2) . . ?
C32 C33 H33 119.2 . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
N3 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C35 H35A 109.5 . . ?
N3 C35 H35B 109.5 . . ?
N3 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C42 121.1(3) . . ?
C41 C36 C37 117.4(3) . . ?
C41 C36 C42 121.5(3) . . ?
C36 C37 H37 119.3 . . ?
C36 C37 C38 121.5(3) . . ?
C38 C37 H37 119.3 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.3(4) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 120.6 . . ?
C40 C39 C38 118.8(3) . . ?
C40 C39 H39 120.6 . . ?
C39 C40 H40 119.5 . . ?
C39 C40 C41 121.0(4) . . ?
C41 C40 H40 119.5 . . ?
C36 C41 C40 121.0(3) . . ?
C36 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C36 C42 H42A 109.5 . . ?
C36 C42 H42B 109.5 . . ?
C36 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C49 116.7(7) . . ?
C48 C43 C44 115.4(8) . . ?
C48 C43 C49 127.9(9) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 C43 120.1(8) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 H45 120.2 . . ?
C44 C45 C46 119.6(10) . . ?
C46 C45 H45 120.2 . . ?
C45 C46 H46 118.7 . . ?
C47 C46 C45 122.5(11) . . ?
C47 C46 H46 118.7 . . ?
C46 C47 H47 120.0 . . ?
C46 C47 C48 119.9(10) . . ?
C48 C47 H47 120.0 . . ?
C43 C48 H48 118.8 . . ?
C47 C48 C43 122.4(9) . . ?
C47 C48 H48 118.8 . . ?
C43 C49 H49A 109.5 . . ?
C43 C49 H49B 109.5 . . ?
C43 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C55 C50 C51 108.1(6) . . ?
C56 C50 C51 133.5(7) . . ?
C56 C50 C55 116.6(7) . . ?
C50 C51 H51 118.5 . . ?
C52 C51 C50 123.0(8) . . ?
C52 C51 H51 118.5 . . ?
C51 C52 H52 118.6 . . ?
C51 C52 C53 122.8(8) . . ?
C53 C52 H52 118.6 . . ?
C52 C53 H53 122.8 . . ?
C54 C53 C52 114.4(8) . . ?
C54 C53 H53 122.8 . . ?
C53 C54 H54 118.1 . . ?
C53 C54 C55 123.8(8) . . ?
C55 C54 H54 118.1 . . ?
C50 C55 H55 117.6 . . ?
C54 C55 C50 124.7(8) . . ?
C54 C55 H55 117.6 . . ?
C50 C56 H56A 109.5 . . ?
C50 C56 H56B 109.5 . . ?
C50 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C28 C29 -136.8(2) . . . . ?
N1 C1 C28 C33 47.1(3) . . . . ?
N1 C2 C3 Cu1 175.86(16) . . . . ?
N1 C2 C3 N2 -0.7(2) . . . . ?
N1 C4 C5 C6 -178.2(2) . . . . ?
N1 C4 C5 C10 -0.8(3) . . . . ?
N1 C4 C9 C8 177.9(2) . . . . ?
N1 C4 C9 C13 -0.3(3) . . . . ?
N2 C1 C28 C29 46.6(3) . . . . ?
N2 C1 C28 C33 -129.4(2) . . . . ?
N2 C16 C17 C18 177.7(2) . . . . ?
N2 C16 C17 C22 -4.0(4) . . . . ?
N2 C16 C21 C20 -177.4(2) . . . . ?
N2 C16 C21 C25 4.8(4) . . . . ?
N3 C31 C32 C33 179.3(2) . . . . ?
C1 N1 C2 C3 0.6(3) . . . . ?
C1 N1 C4 C5 -103.0(3) . . . . ?
C1 N1 C4 C9 80.0(3) . . . . ?
C1 N2 C3 Cu1 -176.03(16) . . . . ?
C1 N2 C3 C2 0.7(2) . . . . ?
C1 N2 C16 C17 -103.6(3) . . . . ?
C1 N2 C16 C21 75.4(3) . . . . ?
C1 C28 C29 C30 -174.9(2) . . . . ?
C1 C28 C33 C32 174.5(2) . . . . ?
C2 N1 C1 N2 -0.1(2) . . . . ?
C2 N1 C1 C28 -177.2(2) . . . . ?
C2 N1 C4 C5 82.1(3) . . . . ?
C2 N1 C4 C9 -95.0(3) . . . . ?
C3 N2 C1 N1 -0.3(2) . . . . ?
C3 N2 C1 C28 176.8(2) . . . . ?
C3 N2 C16 C17 83.1(3) . . . . ?
C3 N2 C16 C21 -97.9(3) . . . . ?
C4 N1 C1 N2 -175.7(2) . . . . ?
C4 N1 C1 C28 7.2(4) . . . . ?
C4 N1 C2 C3 176.3(2) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C4 C5 C10 C11 133.2(3) . . . . ?
C4 C5 C10 C12 -104.2(3) . . . . ?
C4 C9 C13 C14 -121.5(3) . . . . ?
C4 C9 C13 C15 114.1(3) . . . . ?
C5 C4 C9 C8 1.0(4) . . . . ?
C5 C4 C9 C13 -177.1(2) . . . . ?
C5 C6 C7 C8 -0.3(4) . . . . ?
C6 C5 C10 C11 -49.6(3) . . . . ?
C6 C5 C10 C12 73.1(3) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C7 C8 C9 C4 -0.3(4) . . . . ?
C7 C8 C9 C13 177.9(3) . . . . ?
C8 C9 C13 C14 60.4(4) . . . . ?
C8 C9 C13 C15 -64.0(3) . . . . ?
C9 C4 C5 C6 -1.3(3) . . . . ?
C9 C4 C5 C10 176.1(2) . . . . ?
C10 C5 C6 C7 -176.5(2) . . . . ?
C16 N2 C1 N1 -174.35(19) . . . . ?
C16 N2 C1 C28 2.8(3) . . . . ?
C16 N2 C3 Cu1 -2.1(3) . . . . ?
C16 N2 C3 C2 174.6(2) . . . . ?
C16 C17 C18 C19 -0.2(4) . . . . ?
C16 C17 C22 C23 132.2(3) . . . . ?
C16 C17 C22 C24 -105.1(3) . . . . ?
C16 C21 C25 C26 -126.2(3) . . . . ?
C16 C21 C25 C27 110.4(3) . . . . ?
C17 C16 C21 C20 1.6(4) . . . . ?
C17 C16 C21 C25 -176.3(2) . . . . ?
C17 C18 C19 C20 1.2(5) . . . . ?
C18 C17 C22 C23 -49.5(3) . . . . ?
C18 C17 C22 C24 73.1(3) . . . . ?
C18 C19 C20 C21 -0.8(4) . . . . ?
C19 C20 C21 C16 -0.5(4) . . . . ?
C19 C20 C21 C25 177.4(3) . . . . ?
C20 C21 C25 C26 56.0(3) . . . . ?
C20 C21 C25 C27 -67.4(4) . . . . ?
C21 C16 C17 C18 -1.2(4) . . . . ?
C21 C16 C17 C22 177.1(2) . . . . ?
C22 C17 C18 C19 -178.5(3) . . . . ?
C28 C29 C30 C31 0.2(4) . . . . ?
C29 C28 C33 C32 -1.7(4) . . . . ?
C29 C30 C31 N3 -179.8(2) . . . . ?
C29 C30 C31 C32 -1.4(4) . . . . ?
C30 C31 C32 C33 1.0(4) . . . . ?
C31 C32 C33 C28 0.6(4) . . . . ?
C33 C28 C29 C30 1.3(3) . . . . ?
C34 N3 C31 C30 -6.4(4) . . . . ?
C34 N3 C31 C32 175.3(2) . . . . ?
C35 N3 C31 C30 -163.5(2) . . . . ?
C35 N3 C31 C32 18.2(4) . . . . ?
C36 C37 C38 C39 -0.4(6) . . . . ?
C37 C36 C41 C40 0.0(5) . . . . ?
C37 C38 C39 C40 1.2(6) . . . . ?
C38 C39 C40 C41 -1.3(6) . . . . ?
C39 C40 C41 C36 0.7(6) . . . . ?
C41 C36 C37 C38 -0.2(5) . . . . ?
C42 C36 C37 C38 178.0(3) . . . . ?
C42 C36 C41 C40 -178.2(3) . . . . ?
C43 C44 C45 C46 -0.8(15) . . . . ?
C44 C43 C48 C47 0.3(16) . . . . ?
C44 C45 C46 C47 0(2) . . . . ?
C45 C46 C47 C48 1(2) . . . . ?
C46 C47 C48 C43 -1.3(16) . . . . ?
C48 C43 C44 C45 0.7(16) . . . . ?
C49 C43 C44 C45 179.3(10) . . . . ?
C49 C43 C48 C47 -178.1(11) . . . . ?
C50 C51 C52 C53 15.7(14) . . . . ?
C51 C50 C55 C54 14.5(14) . . . . ?
C51 C52 C53 C54 -13.5(14) . . . . ?
C52 C53 C54 C55 12.9(14) . . . . ?
C53 C54 C55 C50 -15.7(15) . . . . ?
C55 C50 C51 C52 -14.9(14) . . . . ?
C56 C50 C51 C52 -178.4(9) . . . . ?
C56 C50 C55 C54 -178.9(9) . . . . ?

_olex2_date_sample_data_collection 2017-06-06
_olex2_date_sample_submission    1496008800
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C42) = Uanis(C49) = Uanis(C56)
Uanis(C48) = Uanis(C44) = Uanis(C37) = Uanis(C41) = Uanis(C51) = Uanis(C55)
Uanis(C53) = Uanis(C39) = Uanis(C46)
Uanis(C38) = Uanis(C40) = Uanis(C45) = Uanis(C47) = Uanis(C52) = Uanis(C54)
3. Same fragment restrains
{C36, C37, C38, C39, C40, C41, C42} sigma for 1-2: 0.02, 1-3: 0.04
as
{C43, C44, C45, C46, C47, C48, C49}
{C36, C37, C38, C39, C40, C41, C42} sigma for 1-2: 0.02, 1-3: 0.04
as
{C50, C51, C52, C53, C54, C55, C56}
4. Others
 Fixed Sof: C43(0.5) C44(0.5) H44(0.5) C45(0.5) H45(0.5) C46(0.5) H46(0.5)
 C47(0.5) H47(0.5) C48(0.5) H48(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5)
 C50(0.5) C51(0.5) H51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5)
 H54(0.5) C55(0.5) H55(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29),
 C30(H30), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C),
 C49(H49A,H49B,H49C), C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.420
_oxdiff_exptl_absorpt_empirical_full_min 0.523

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_SHELXL_version_number     2016/4
_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.
;
