# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_pv213_c
_database_code_depnum_ccdc_archive 'CCDC 2094731'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2020-11-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H36 Cl N2 O3 Rh'
_chemical_formula_sum            'C31 H36 Cl N2 O3 Rh'
_chemical_formula_weight         622.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H36 N2 O3 Cl1 Rh1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.32987(14)
_cell_length_b                   14.7730(2)
_cell_length_c                   20.5303(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.0954(13)
_cell_angle_gamma                90
_cell_volume                     3093.59(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4480
_cell_measurement_theta_min      3.6780
_shelx_estimated_absorpt_T_max   0.490
_shelx_estimated_absorpt_T_min   0.422
_exptl_absorpt_coefficient_mu    5.509
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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 pale yellow'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 -1 0.0824
-1 -1 0 0.1008
-1 -2 -2 0.1055
-1 0 1 0.0666
1 0 -1 0.0990
1 2 2 0.0760
1 -2 -1 0.1017
0 -1 -1 0.1052
2 -1 1 0.0963
-2 1 -1 0.0848
-1 2 1 0.0880
0 1 1 0.0697
1 -1 1 0.0903
0 -2 13 0.0544
-1 -9 4 0.0870
-1 0 5 0.0519
-3 -5 3 0.0886
2 2 -5 0.0802
1 2 -5 0.0707
2 5 2 0.0709

_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.151
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
2.0000 1.0000 -1.0000 0.2625 -0.1167 -0.1343
-1.0000 -1.0000 -0.0000 -0.1138 0.0641 0.1290
-1.0000 -2.0000 -2.0000 -0.0705 0.0185 0.3023
-1.0000 -0.0000 1.0000 -0.1488 0.0527 0.0053
1.0000 0.0000 -1.0000 0.1488 -0.0527 -0.0053
1.0000 2.0000 2.0000 0.0705 -0.0185 -0.3023
1.0000 -2.0000 -1.0000 0.2025 0.0841 0.1428
0.0000 -1.0000 -1.0000 0.0350 0.0114 0.1237
2.0000 -1.0000 1.0000 0.2999 0.1339 -0.0855
-2.0000 1.0000 -1.0000 -0.2999 -0.1339 0.0855
-1.0000 2.0000 1.0000 -0.2025 -0.0841 -0.1428
-0.0000 1.0000 1.0000 -0.0350 -0.0114 -0.1237
1.0000 -1.0000 1.0000 0.1593 0.1296 -0.0305
0.4528 -2.2926 12.6041 0.0219 0.8766 -0.4807
-1.3165 -8.9956 4.1649 0.0223 0.8466 0.5318
-1.0000 -0.0000 5.0000 -0.1816 0.2805 -0.1932
-3.0000 -5.0001 3.0000 -0.3122 0.4998 0.3862
2.0000 2.0000 -5.0000 0.2685 -0.4129 -0.0098
1.0000 2.0000 -5.0000 0.1279 -0.4172 0.0451
2.0000 5.0000 2.0000 0.1306 -0.2193 -0.5794

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15548
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.620
_diffrn_reflns_theta_min         3.702
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -12.00   1.00    1.00    --  -40.91 -60.00 178.00   97
  2  ω    -11.00  32.00   1.00    1.00    --  -40.91  60.00 -41.00   43
  3  ω    -56.00 -21.00   1.00    1.00    --  -40.91  60.00 -41.00   35
  4  ω     -5.00  20.00   1.00    1.00    --   40.91 -60.00 178.00   25
  5  ω     87.00 175.00   1.00    4.00    --  105.15  60.00 -41.00   88
  6  ω     35.00 130.00   1.00    4.00    --  105.15 -60.00 178.00   95
  7  ω     37.00  85.00   1.00    1.00    --   40.91-125.00 120.00   48
  8  ω     30.00  96.00   1.00    1.00    --   40.91-125.00  30.00   66
  9  ω     17.00  45.00   1.00    1.00    --   40.91 -99.00-180.00   28
 10  ω     38.00  63.00   1.00    1.00    --   40.91  60.00 -41.00   25
 11  ω    103.00 171.00   1.00    4.00    --  105.15  77.00  30.00   68
 12  ω     96.00 146.00   1.00    4.00    --  105.15 178.00  90.00   50
 13  ω    104.00 158.00   1.00    4.00    --  105.15  77.00   0.00   54
 14  ω    103.00 168.00   1.00    4.00    --  105.15  77.00 -90.00   65
 15  ω    113.00 168.00   1.00    4.00    --  105.15 111.00-150.00   55
 16  ω    135.00 174.00   1.00    4.00    --  105.15 111.00-120.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1406012000
_diffrn_orient_matrix_UB_12      -0.0268471000
_diffrn_orient_matrix_UB_13      -0.0081970000
_diffrn_orient_matrix_UB_21      0.0043013000
_diffrn_orient_matrix_UB_22      -0.0683677000
_diffrn_orient_matrix_UB_23      0.0569604000
_diffrn_orient_matrix_UB_31      -0.0549414000
_diffrn_orient_matrix_UB_32      -0.0740562000
_diffrn_orient_matrix_UB_33      -0.0496332000
_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                5408
_reflns_number_total             6015
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.057
_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     351
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0278
_refine_ls_restrained_S_all      1.044
_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)+(0.0255P)²+2.0812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0683
_refine_special_details          ?
_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)
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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.47631(2) 0.40184(2) 0.64021(2) 0.02805(6) Uani 1 1 d . . . . .
Cl1 Cl 0.38003(6) 0.30653(4) 0.71039(3) 0.04233(14) Uani 1 1 d . . . . .
O1 O 0.76451(16) 0.41000(12) 0.76118(9) 0.0415(4) Uani 1 1 d . . . . .
O2 O 0.6159(2) 0.52348(15) 0.55896(9) 0.0567(5) Uani 1 1 d . . . . .
O3 O 0.3760(3) 0.27869(19) 0.52775(12) 0.0887(9) Uani 1 1 d . . . . .
N1 N 0.35656(16) 0.57335(12) 0.73861(8) 0.0230(3) Uani 1 1 d . . . . .
N2 N 0.48757(16) 0.54123(12) 0.82907(8) 0.0229(3) Uani 1 1 d . . . . .
C1 C 0.46861(18) 0.52856(13) 0.76307(9) 0.0208(4) Uani 1 1 d . . . . .
C2 C 0.3886(2) 0.59552(15) 0.84598(11) 0.0302(5) Uani 1 1 d . . . . .
H2 H 0.379732 0.615062 0.889141 0.036 Uiso 1 1 calc R U . . .
C3 C 0.3075(2) 0.61535(16) 0.79004(11) 0.0304(5) Uani 1 1 d . . . . .
H3 H 0.230597 0.651506 0.786342 0.036 Uiso 1 1 calc R U . . .
C4 C 0.3113(2) 0.58856(14) 0.66896(10) 0.0253(4) Uani 1 1 d . . . . .
C5 C 0.3755(2) 0.65497(15) 0.63760(11) 0.0278(4) Uani 1 1 d . . . . .
C6 C 0.3370(2) 0.66494(17) 0.56972(11) 0.0336(5) Uani 1 1 d . . . . .
H6 H 0.379404 0.708666 0.546515 0.040 Uiso 1 1 calc R U . . .
C7 C 0.2382(2) 0.61236(17) 0.53569(11) 0.0365(5) Uani 1 1 d . . . . .
H7 H 0.215002 0.618955 0.489288 0.044 Uiso 1 1 calc R U . . .
C8 C 0.1731(2) 0.55016(17) 0.56900(12) 0.0366(5) Uani 1 1 d . . . . .
H8 H 0.103508 0.515833 0.545160 0.044 Uiso 1 1 calc R U . . .
C9 C 0.2070(2) 0.53660(15) 0.63660(11) 0.0292(4) Uani 1 1 d . . . . .
C10 C 0.1263(2) 0.47473(17) 0.67356(13) 0.0373(5) Uani 1 1 d . . . . .
H10 H 0.183583 0.453513 0.714568 0.045 Uiso 1 1 calc R U . . .
C11 C 0.0737(3) 0.3913(2) 0.63373(16) 0.0537(8) Uani 1 1 d . . . . .
H11A H 0.007973 0.410103 0.596431 0.080 Uiso 1 1 calc R U . . .
H11B H 0.033532 0.349943 0.662033 0.080 Uiso 1 1 calc R U . . .
H11C H 0.146088 0.360547 0.617219 0.080 Uiso 1 1 calc R U . . .
C12 C 0.0130(3) 0.5289(2) 0.69396(17) 0.0548(8) Uani 1 1 d . . . . .
H12A H 0.047827 0.581628 0.719893 0.082 Uiso 1 1 calc R U . . .
H12B H -0.035726 0.490513 0.720617 0.082 Uiso 1 1 calc R U . . .
H12C H -0.045781 0.549091 0.654438 0.082 Uiso 1 1 calc R U . . .
C13 C 0.4782(2) 0.71816(17) 0.67430(11) 0.0342(5) Uani 1 1 d . . . . .
H13 H 0.499153 0.696104 0.720824 0.041 Uiso 1 1 calc R U . . .
C14 C 0.6036(3) 0.7200(2) 0.6464(2) 0.0696(11) Uani 1 1 d . . . . .
H14A H 0.641026 0.658970 0.647708 0.104 Uiso 1 1 calc R U . . .
H14B H 0.665831 0.761093 0.672579 0.104 Uiso 1 1 calc R U . . .
H14C H 0.586159 0.741279 0.600621 0.104 Uiso 1 1 calc R U . . .
C15 C 0.4227(3) 0.8134(2) 0.6762(2) 0.0674(10) Uani 1 1 d . . . . .
H15A H 0.402788 0.837361 0.631223 0.101 Uiso 1 1 calc R U . . .
H15B H 0.487369 0.852539 0.702688 0.101 Uiso 1 1 calc R U . . .
H15C H 0.342382 0.811680 0.695945 0.101 Uiso 1 1 calc R U . . .
C16 C 0.6014(2) 0.50958(15) 0.87299(9) 0.0257(4) Uani 1 1 d . . . . .
C17 C 0.7129(2) 0.56475(17) 0.88119(11) 0.0331(5) Uani 1 1 d . . . . .
C18 C 0.8217(3) 0.5327(2) 0.92369(14) 0.0463(6) Uani 1 1 d . . . . .
H18 H 0.899393 0.568161 0.931063 0.056 Uiso 1 1 calc R U . . .
C19 C 0.8188(3) 0.4511(2) 0.95508(15) 0.0563(8) Uani 1 1 d . . . . .
H19 H 0.894572 0.430765 0.983714 0.068 Uiso 1 1 calc R U . . .
C20 C 0.7075(3) 0.39799(19) 0.94569(14) 0.0462(6) Uani 1 1 d . . . . .
H20 H 0.707626 0.341575 0.967909 0.055 Uiso 1 1 calc R U . . .
C21 C 0.5950(2) 0.42600(16) 0.90411(11) 0.0310(5) Uani 1 1 d . . . . .
C22 C 0.4720(2) 0.36816(16) 0.89454(11) 0.0343(5) Uani 1 1 d . . . . .
H22 H 0.413240 0.390561 0.854352 0.041 Uiso 1 1 calc R U . . .
C23 C 0.5009(3) 0.26831(18) 0.88376(16) 0.0528(7) Uani 1 1 d . . . . .
H23A H 0.550969 0.262576 0.847210 0.079 Uiso 1 1 calc R U . . .
H23B H 0.418201 0.235004 0.873140 0.079 Uiso 1 1 calc R U . . .
H23C H 0.552064 0.243314 0.924003 0.079 Uiso 1 1 calc R U . . .
C24 C 0.3998(3) 0.3803(2) 0.95356(15) 0.0586(8) Uani 1 1 d . . . . .
H24A H 0.456515 0.360485 0.993881 0.088 Uiso 1 1 calc R U . . .
H24B H 0.319529 0.343823 0.946923 0.088 Uiso 1 1 calc R U . . .
H24C H 0.377202 0.444203 0.957665 0.088 Uiso 1 1 calc R U . . .
C25 C 0.7188(2) 0.65497(18) 0.84683(12) 0.0388(6) Uani 1 1 d . . . . .
H25 H 0.634501 0.662358 0.815830 0.047 Uiso 1 1 calc R U . . .
C26 C 0.8292(4) 0.6589(2) 0.80591(17) 0.0660(10) Uani 1 1 d . . . . .
H26A H 0.913626 0.652636 0.834950 0.099 Uiso 1 1 calc R U . . .
H26B H 0.826356 0.717156 0.782833 0.099 Uiso 1 1 calc R U . . .
H26C H 0.818737 0.609623 0.773591 0.099 Uiso 1 1 calc R U . . .
C27 C 0.7291(3) 0.73346(19) 0.89553(14) 0.0482(6) Uani 1 1 d . . . . .
H27A H 0.653800 0.732254 0.919212 0.072 Uiso 1 1 calc R U . . .
H27B H 0.729647 0.790785 0.871558 0.072 Uiso 1 1 calc R U . . .
H27C H 0.810301 0.727825 0.927146 0.072 Uiso 1 1 calc R U . . .
C28 C 0.54814(19) 0.47909(14) 0.72613(9) 0.0230(4) Uani 1 1 d . . . . .
C29 C 0.6616(2) 0.44400(15) 0.74835(10) 0.0271(4) Uani 1 1 d . . . . .
C30 C 0.5609(3) 0.47725(18) 0.58918(11) 0.0388(5) Uani 1 1 d . . . . .
C31 C 0.4138(3) 0.3267(2) 0.56939(14) 0.0525(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Cl1 2.3454(6) . ?
Rh1 C28 2.133(2) . ?
Rh1 C30 1.842(3) . ?
Rh1 C31 1.862(3) . ?
O1 C29 1.167(3) . ?
O2 C30 1.134(3) . ?
O3 C31 1.131(3) . ?
N1 C1 1.359(3) . ?
N1 C3 1.388(3) . ?
N1 C4 1.450(3) . ?
N2 C1 1.351(3) . ?
N2 C2 1.386(3) . ?
N2 C16 1.442(3) . ?
C1 C28 1.407(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.342(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.397(3) . ?
C4 C9 1.402(3) . ?
C5 C6 1.395(3) . ?
C5 C13 1.520(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.391(3) . ?
C9 C10 1.519(3) . ?
C10 H10 1.0000 . ?
C10 C11 1.530(4) . ?
C10 C12 1.529(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.497(4) . ?
C13 C15 1.522(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.400(3) . ?
C16 C21 1.397(3) . ?
C17 C18 1.392(3) . ?
C17 C25 1.514(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.370(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.381(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.391(3) . ?
C21 C22 1.518(3) . ?
C22 H22 1.0000 . ?
C22 C23 1.528(4) . ?
C22 C24 1.530(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 1.0000 . ?
C25 C26 1.521(4) . ?
C25 C27 1.524(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.297(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C28 Rh1 Cl1 86.51(6) . . ?
C30 Rh1 Cl1 176.41(8) . . ?
C30 Rh1 C28 90.71(9) . . ?
C30 Rh1 C31 93.09(12) . . ?
C31 Rh1 Cl1 89.61(10) . . ?
C31 Rh1 C28 175.61(11) . . ?
C1 N1 C3 109.20(17) . . ?
C1 N1 C4 124.26(17) . . ?
C3 N1 C4 125.56(17) . . ?
C1 N2 C2 109.61(17) . . ?
C1 N2 C16 123.84(17) . . ?
C2 N2 C16 126.30(17) . . ?
N1 C1 C28 126.11(18) . . ?
N2 C1 N1 106.45(17) . . ?
N2 C1 C28 127.44(18) . . ?
N2 C2 H2 126.4 . . ?
C3 C2 N2 107.30(18) . . ?
C3 C2 H2 126.4 . . ?
N1 C3 H3 126.3 . . ?
C2 C3 N1 107.44(18) . . ?
C2 C3 H3 126.3 . . ?
C5 C4 N1 117.44(18) . . ?
C5 C4 C9 123.5(2) . . ?
C9 C4 N1 119.09(19) . . ?
C4 C5 C13 123.20(19) . . ?
C6 C5 C4 116.9(2) . . ?
C6 C5 C13 119.8(2) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(2) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.1(2) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.2 . . ?
C7 C8 C9 121.6(2) . . ?
C9 C8 H8 119.2 . . ?
C4 C9 C10 122.3(2) . . ?
C8 C9 C4 116.6(2) . . ?
C8 C9 C10 120.9(2) . . ?
C9 C10 H10 108.1 . . ?
C9 C10 C11 113.2(2) . . ?
C9 C10 C12 109.1(2) . . ?
C11 C10 H10 108.1 . . ?
C12 C10 H10 108.1 . . ?
C12 C10 C11 110.2(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 . . ?
C5 C13 H13 107.6 . . ?
C5 C13 C15 110.1(2) . . ?
C14 C13 C5 113.6(2) . . ?
C14 C13 H13 107.6 . . ?
C14 C13 C15 110.2(3) . . ?
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 117.4(2) . . ?
C21 C16 N2 118.72(19) . . ?
C21 C16 C17 123.8(2) . . ?
C16 C17 C25 123.3(2) . . ?
C18 C17 C16 116.4(2) . . ?
C18 C17 C25 120.2(2) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 C17 121.3(3) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 H19 119.5 . . ?
C18 C19 C20 120.9(2) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.9(3) . . ?
C21 C20 H20 119.6 . . ?
C16 C21 C22 122.48(19) . . ?
C20 C21 C16 116.7(2) . . ?
C20 C21 C22 120.8(2) . . ?
C21 C22 H22 107.9 . . ?
C21 C22 C23 112.5(2) . . ?
C21 C22 C24 109.5(2) . . ?
C23 C22 H22 107.9 . . ?
C23 C22 C24 111.0(2) . . ?
C24 C22 H22 107.9 . . ?
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 . . ?
C17 C25 H25 107.3 . . ?
C17 C25 C26 112.3(2) . . ?
C17 C25 C27 111.6(2) . . ?
C26 C25 H25 107.3 . . ?
C26 C25 C27 110.6(2) . . ?
C27 C25 H25 107.3 . . ?
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 . . ?
C1 C28 Rh1 124.54(14) . . ?
C29 C28 Rh1 104.71(15) . . ?
C29 C28 C1 126.17(19) . . ?
O1 C29 C28 172.5(2) . . ?
O2 C30 Rh1 178.2(3) . . ?
O3 C31 Rh1 177.8(3) . . ?

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 Rh1 -35.2(3) . . . . ?
N1 C1 C28 C29 172.6(2) . . . . ?
N1 C4 C5 C6 175.92(19) . . . . ?
N1 C4 C5 C13 -7.2(3) . . . . ?
N1 C4 C9 C8 -176.1(2) . . . . ?
N1 C4 C9 C10 9.3(3) . . . . ?
N2 C1 C28 Rh1 144.89(17) . . . . ?
N2 C1 C28 C29 -7.4(4) . . . . ?
N2 C2 C3 N1 -0.1(3) . . . . ?
N2 C16 C17 C18 -179.9(2) . . . . ?
N2 C16 C17 C25 0.4(3) . . . . ?
N2 C16 C21 C20 179.6(2) . . . . ?
N2 C16 C21 C22 -1.3(3) . . . . ?
C1 N1 C3 C2 -0.6(3) . . . . ?
C1 N1 C4 C5 -75.3(3) . . . . ?
C1 N1 C4 C9 104.5(2) . . . . ?
C1 N2 C2 C3 0.7(3) . . . . ?
C1 N2 C16 C17 84.6(3) . . . . ?
C1 N2 C16 C21 -94.6(2) . . . . ?
C2 N2 C1 N1 -1.1(2) . . . . ?
C2 N2 C1 C28 178.8(2) . . . . ?
C2 N2 C16 C17 -88.9(3) . . . . ?
C2 N2 C16 C21 91.8(3) . . . . ?
C3 N1 C1 N2 1.1(2) . . . . ?
C3 N1 C1 C28 -178.9(2) . . . . ?
C3 N1 C4 C5 92.1(3) . . . . ?
C3 N1 C4 C9 -88.1(3) . . . . ?
C4 N1 C1 N2 170.23(18) . . . . ?
C4 N1 C1 C28 -9.7(3) . . . . ?
C4 N1 C3 C2 -169.6(2) . . . . ?
C4 C5 C6 C7 1.1(3) . . . . ?
C4 C5 C13 C14 128.1(3) . . . . ?
C4 C5 C13 C15 -107.8(3) . . . . ?
C4 C9 C10 C11 -148.8(2) . . . . ?
C4 C9 C10 C12 88.1(3) . . . . ?
C5 C4 C9 C8 3.7(3) . . . . ?
C5 C4 C9 C10 -170.9(2) . . . . ?
C5 C6 C7 C8 1.8(4) . . . . ?
C6 C5 C13 C14 -55.1(3) . . . . ?
C6 C5 C13 C15 69.0(3) . . . . ?
C6 C7 C8 C9 -2.0(4) . . . . ?
C7 C8 C9 C4 -0.6(4) . . . . ?
C7 C8 C9 C10 174.1(2) . . . . ?
C8 C9 C10 C11 36.8(3) . . . . ?
C8 C9 C10 C12 -86.3(3) . . . . ?
C9 C4 C5 C6 -3.9(3) . . . . ?
C9 C4 C5 C13 173.0(2) . . . . ?
C13 C5 C6 C7 -175.9(2) . . . . ?
C16 N2 C1 N1 -175.57(18) . . . . ?
C16 N2 C1 C28 4.4(3) . . . . ?
C16 N2 C2 C3 175.0(2) . . . . ?
C16 C17 C18 C19 0.5(4) . . . . ?
C16 C17 C25 C26 -123.1(3) . . . . ?
C16 C17 C25 C27 111.9(3) . . . . ?
C16 C21 C22 C23 135.6(2) . . . . ?
C16 C21 C22 C24 -100.4(3) . . . . ?
C17 C16 C21 C20 0.4(3) . . . . ?
C17 C16 C21 C22 179.5(2) . . . . ?
C17 C18 C19 C20 -0.2(5) . . . . ?
C18 C17 C25 C26 57.1(3) . . . . ?
C18 C17 C25 C27 -67.8(3) . . . . ?
C18 C19 C20 C21 -0.1(5) . . . . ?
C19 C20 C21 C16 0.0(4) . . . . ?
C19 C20 C21 C22 -179.1(3) . . . . ?
C20 C21 C22 C23 -45.3(3) . . . . ?
C20 C21 C22 C24 78.7(3) . . . . ?
C21 C16 C17 C18 -0.6(3) . . . . ?
C21 C16 C17 C25 179.6(2) . . . . ?
C25 C17 C18 C19 -179.7(3) . . . . ?

_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.447
_oxdiff_exptl_absorpt_empirical_full_min 0.824
####################################################################### 
# 
# 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_wf446hcl
_database_code_depnum_ccdc_archive 'CCDC 2094061'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-07-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C58 H72 N4 O2'
_chemical_formula_sum            'C58 H72 N4 O2'
_chemical_formula_weight         857.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C58 H72 N4 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   21.7877(2)
_cell_length_b                   12.66021(12)
_cell_length_c                   37.7430(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.9129(10)
_cell_angle_gamma                90
_cell_volume                     10255.47(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19442
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.8640
_cell_measurement_theta_min      3.6570
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.752
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3712
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0384
-1 0 0 0.0787
0 1 0 0.1521
0 -2 -1 0.2476
0 -1 -2 0.1749
0 0 -1 0.2622
0 0 1 0.1941
0 1 2 0.2151
-1 -1 2 0.2917
1 0 -1 0.1160
1 0 2 0.1392
2 -1 0 0.1959
0 -1 2 0.2862

_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.12
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
1.0001 -0.0002 0.0008 0.0708 0.0062 0.0100
-1.0001 0.0002 -0.0008 -0.0708 -0.0062 -0.0100
-0.0000 1.0002 0.0004 0.0065 -0.1186 0.0267
-0.0009 -2.0002 -1.0006 -0.0265 0.2450 -0.0150
-0.0018 -0.9997 -2.0001 -0.0334 0.1343 0.0501
-0.0009 0.0003 -0.9999 -0.0134 0.0079 0.0384
0.0009 -0.0003 0.9999 0.0134 -0.0079 -0.0384
0.0018 0.9997 2.0001 0.0334 -0.1343 -0.0501
-0.9982 -1.0005 1.9985 -0.0505 0.0966 -0.1135
0.9992 0.0000 -0.9990 0.0574 0.0141 0.0484
1.0019 -0.0008 2.0006 0.0977 -0.0096 -0.0668
2.0002 -1.0007 0.0013 0.1351 0.1309 -0.0067
0.0019 -1.0008 1.9994 0.0204 0.1028 -0.1035

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            60758
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.063
_diffrn_reflns_theta_min         3.688
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  33.00   1.00    1.00    --  -41.04  29.00  50.00   96
  2  ω   -118.00 -28.00   1.00    1.00    --  -41.04 -29.00-110.00   90
  3  ω     87.00 117.00   1.00    1.00    --   41.04  29.00  50.00   30
  4  ω     41.00  89.00   1.00    1.00    --  112.00 -29.00-110.00   48
  5  ω     92.00 122.00   1.00    1.00    --  112.00 -29.00-110.00   30
  6  ω    114.00 178.00   1.00    1.00    --  112.00  29.00  50.00   64
  7  ω    -58.00  -9.00   1.00    1.00    --  -41.04 125.00  60.00   49
  8  ω    -20.00  70.00   1.00    1.00    --   41.04 -77.00-180.00   90
  9  ω     56.00  96.00   1.00    1.00    --   41.04-125.00 -90.00   40
 10  ω     -8.00  17.00   1.00    1.00    --   41.04 -29.00-110.00   25
 11  ω     30.00  85.00   1.00    1.00    --   41.04-125.00  90.00   55
 12  ω     29.00  74.00   1.00    1.00    --  112.00 -94.00-120.00   45
 13  ω     90.00 124.00   1.00    1.00    --  112.00  45.00 -90.00   34
 14  ω     41.00 141.00   1.00    1.00    --  112.00 -61.00   0.00  100
 15  ω    137.00 163.00   1.00    1.00    --  112.00 111.00-180.00   26
 16  ω     62.00 138.00   1.00    1.00    --  112.00 178.00-120.00   76
 17  ω    142.00 178.00   1.00    1.00    --  112.00  30.00 150.00   36
 18  ω    127.00 171.00   1.00    1.00    --  112.00  45.00  90.00   44
 19  ω    105.00 147.00   1.00    1.00    --  112.00 111.00 -30.00   42
 20  ω     48.00 141.00   1.00    1.00    --  112.00 -61.00 -90.00   93
 21  ω     70.00 106.00   1.00    1.00    --  112.00 -94.00 -60.00   36
 22  ω     46.00  71.00   1.00    1.00    --  112.00-111.00  60.00   25
 23  ω     36.00  73.00   1.00    1.00    --  112.00 -94.00-150.00   37
 24  ω     84.00 109.00   1.00    1.00    --  112.00-111.00 120.00   25
 25  ω     76.00 109.00   1.00    1.00    --  112.00-111.00  60.00   33
 26  ω    104.00 130.00   1.00    1.00    --  112.00 111.00-180.00   26
 27  ω     81.00 109.00   1.00    1.00    --  112.00-111.00-150.00   28
 28  ω     85.00 129.00   1.00    1.00    --  112.00  30.00 150.00   44
 29  ω    150.00 178.00   1.00    1.00    --  112.00  15.00 120.00   28
 30  ω     45.00 149.00   1.00    1.00    --  112.00 -15.00  90.00  104
 31  ω     59.00 109.00   1.00    1.00    --  112.00-111.00   0.00   50
 32  ω     73.00 109.00   1.00    1.00    --  112.00-111.00 150.00   36
 33  ω     66.00 109.00   1.00    1.00    --  112.00-111.00 -90.00   43
 34  ω     82.00 107.00   1.00    1.00    --  112.00-111.00  90.00   25
 35  ω     59.00 129.00   1.00    1.00    --  112.00  15.00 120.00   70
 36  ω     36.00 102.00   1.00    1.00    --  112.00-111.00 -60.00   66
 37  ω     49.00  75.00   1.00    1.00    --  112.00-111.00-150.00   26
 38  ω     40.00  65.00   1.00    1.00    --  112.00-111.00 120.00   25
 39  ω     76.00 107.00   1.00    1.00    --  112.00-111.00-120.00   31
 40  ω     59.00 107.00   1.00    1.00    --  112.00-111.00  30.00   48
 41  ω     37.00  63.00   1.00    1.00    --  112.00 -94.00 -60.00   26
 42  ω     31.00  56.00   1.00    1.00    --  112.00 -94.00  90.00   25
 43  ω     48.00  84.00   1.00    1.00    --  112.00 -94.00-180.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0708032000
_diffrn_orient_matrix_UB_12      0.0065231000
_diffrn_orient_matrix_UB_13      0.0133844000
_diffrn_orient_matrix_UB_21      0.0061543000
_diffrn_orient_matrix_UB_22      -0.1185337000
_diffrn_orient_matrix_UB_23      -0.0079311000
_diffrn_orient_matrix_UB_31      0.0100509000
_diffrn_orient_matrix_UB_32      0.0267282000
_diffrn_orient_matrix_UB_33      -0.0384082000
_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                9079
_reflns_number_total             10659
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.000248(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         10659
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.044
_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)+(0.0615P)²+5.9839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1232
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21A-C19 \\sim C21B-C19 \\sim C20A-C19 \\sim C20B-C19
 with sigma of 0.01
 C48A-C46 \\sim C48B-C46 \\sim C47A-C46 \\sim C47B-C46
 with sigma of 0.02
 C47A-C48A \\sim C47B-C48B
 with sigma of 0.02
 C59B-C60B \\sim C60A-C59A
 with sigma of 0.02
 C59B-C58B \\sim C59A-C58A \\sim C60B-C58B \\sim C60A-C58A
 with sigma of 0.01
 C58B-C54 \\sim C54-C58A
 with sigma of 0.01
 C21A-C20A \\sim C21B-C20B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C46 \\sim C47A \\sim C47B \\sim C48A \\sim C48B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C19 \\sim C20A \\sim C20B \\sim C21A \\sim C21B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C58A \\sim C58B \\sim C59A \\sim C59B \\sim C60A \\sim C60B: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C58B)=Sof(H58B)=Sof(C59B)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C60B)=
 Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60A)=
 Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
 Sof(H46A)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48B)=Sof(H48D)=
 Sof(H48E)=Sof(H48F)=1-FVAR(2)
 Sof(H46)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48A)=Sof(H48A)=
 Sof(H48B)=Sof(H48C)=FVAR(2)
 Sof(H19A)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21B)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=1-FVAR(3)
 Sof(H19)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21A)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C19(H19A), C22(H22), C31(H31), C34(H34), C43(H43), C46(H46),
 C46(H46A), C55(H55), C58A(H58A), C58B(H58B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C27(H27),
 C28(H28), C29(H29), C39(H39), C40(H40), C41(H41), C51(H51), C52(H52), C53(H53)
5.c Idealised Me refined as rotating group:
 C20A(H20A,H20B,H20C), C20B(H20D,H20E,H20F), C21A(H21A,H21B,H21C), C21B(H21D,
 H21E,H21F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F),
 C48A(H48A,H48B,H48C), C48B(H48D,H48E,H48F), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C59A(H59A,H59B,H59C), C59B(H59D,H59E,H59F), C60A(H60A,H60B,H60C),
 C60B(H60D,H60E,H60F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.43838(4) 0.11690(7) 0.38320(4) 0.0486(3) Uani 1 1 d . . . . .
O2 O 0.46794(4) 0.46241(7) 0.36250(3) 0.0433(3) Uani 1 1 d . . . . .
N1 N 0.29324(4) 0.25391(7) 0.35822(3) 0.0223(2) Uani 1 1 d . . . . .
N2 N 0.31384(4) 0.42304(7) 0.36013(3) 0.0218(2) Uani 1 1 d . . . . .
N3 N 0.59967(5) 0.17389(8) 0.39279(3) 0.0295(2) Uani 1 1 d . . . . .
N4 N 0.60952(5) 0.33618(8) 0.37478(3) 0.0276(2) Uani 1 1 d . . . . .
C2 C 0.34185(5) 0.32472(8) 0.36360(3) 0.0194(2) Uani 1 1 d . . . . .
C4 C 0.24941(5) 0.41106(9) 0.35217(3) 0.0256(2) Uani 1 1 d . . . . .
H4 H 0.219641 0.466532 0.348309 0.031 Uiso 1 1 calc R U . . .
C5 C 0.23692(5) 0.30792(10) 0.35092(3) 0.0260(2) Uani 1 1 d . . . . .
H5 H 0.196666 0.276837 0.345937 0.031 Uiso 1 1 calc R U . . .
C6 C 0.40501(5) 0.30349(9) 0.37006(3) 0.0212(2) Uani 1 1 d . . . . .
C7 C 0.44646(5) 0.21030(9) 0.37834(3) 0.0256(2) Uani 1 1 d . . . . .
C8 C 0.46034(5) 0.36963(9) 0.36888(3) 0.0245(2) Uani 1 1 d . . . . .
C9 C 0.50215(5) 0.27772(9) 0.37778(3) 0.0224(2) Uani 1 1 d . . . . .
C10 C 0.56584(5) 0.26311(9) 0.38156(3) 0.0237(2) Uani 1 1 d . . . . .
C11 C 0.66265(6) 0.19237(11) 0.39268(4) 0.0391(3) Uani 1 1 d . . . . .
H11 H 0.695512 0.143178 0.399409 0.047 Uiso 1 1 calc R U . . .
C12 C 0.66879(6) 0.29082(11) 0.38153(4) 0.0370(3) Uani 1 1 d . . . . .
H12 H 0.706665 0.324247 0.378667 0.044 Uiso 1 1 calc R U . . .
C13 C 0.29756(5) 0.14053(9) 0.35930(3) 0.0257(2) Uani 1 1 d . . . . .
C14 C 0.30172(6) 0.08678(10) 0.32749(4) 0.0327(3) Uani 1 1 d . . . . .
C15 C 0.30387(7) -0.02316(11) 0.32895(5) 0.0433(3) Uani 1 1 d . . . . .
H15 H 0.306517 -0.062228 0.307780 0.052 Uiso 1 1 calc R U . . .
C16 C 0.30220(7) -0.07601(11) 0.36070(5) 0.0459(4) Uani 1 1 d . . . . .
H16 H 0.303783 -0.150991 0.361214 0.055 Uiso 1 1 calc R U . . .
C17 C 0.29826(6) -0.02076(11) 0.39173(4) 0.0407(3) Uani 1 1 d . . . . .
H17 H 0.297708 -0.058349 0.413454 0.049 Uiso 1 1 calc R U . . .
C18 C 0.29508(6) 0.08921(10) 0.39179(4) 0.0317(3) Uani 1 1 d . . . . .
C19 C 0.30373(7) 0.14452(12) 0.29260(4) 0.0422(3) Uani 1 1 d D U . . .
H19 H 0.293219 0.220252 0.296127 0.051 Uiso 0.689(12) 1 calc R U P A 1
H19A H 0.309044 0.221746 0.297796 0.051 Uiso 0.311(12) 1 calc R U P A 2
C20A C 0.2583(3) 0.1029(4) 0.26060(12) 0.0643(12) Uani 0.689(12) 1 d D U P A 1
H20A H 0.261572 0.145338 0.239287 0.096 Uiso 0.689(12) 1 calc R U P A 1
H20B H 0.215765 0.107381 0.265674 0.096 Uiso 0.689(12) 1 calc R U P A 1
H20C H 0.268277 0.029099 0.256173 0.096 Uiso 0.689(12) 1 calc R U P A 1
C20B C 0.2384(4) 0.1261(9) 0.2690(3) 0.062(2) Uani 0.311(12) 1 d D U P A 2
H20D H 0.237846 0.156369 0.245089 0.093 Uiso 0.311(12) 1 calc R U P A 2
H20E H 0.206397 0.160200 0.280387 0.093 Uiso 0.311(12) 1 calc R U P A 2
H20F H 0.230068 0.050096 0.266844 0.093 Uiso 0.311(12) 1 calc R U P A 2
C21A C 0.37109(17) 0.1403(5) 0.28411(12) 0.0620(11) Uani 0.689(12) 1 d D U P A
1
H21A H 0.382460 0.066804 0.280322 0.093 Uiso 0.689(12) 1 calc R U P A 1
H21B H 0.400204 0.170136 0.304326 0.093 Uiso 0.689(12) 1 calc R U P A 1
H21C H 0.373038 0.181414 0.262321 0.093 Uiso 0.689(12) 1 calc R U P A 1
C21B C 0.3552(6) 0.1082(9) 0.2736(3) 0.068(2) Uani 0.311(12) 1 d D U P A 2
H21D H 0.346808 0.035849 0.264914 0.102 Uiso 0.311(12) 1 calc R U P A 2
H21E H 0.394942 0.110243 0.290336 0.102 Uiso 0.311(12) 1 calc R U P A 2
H21F H 0.357467 0.154992 0.253169 0.102 Uiso 0.311(12) 1 calc R U P A 2
C22 C 0.28920(7) 0.14869(12) 0.42595(4) 0.0416(3) Uani 1 1 d . . . . .
H22 H 0.281545 0.224707 0.419463 0.050 Uiso 1 1 calc R U . . .
C23 C 0.34968(10) 0.1422(2) 0.45308(5) 0.0711(6) Uani 1 1 d . . . . .
H23A H 0.359690 0.068016 0.458803 0.107 Uiso 1 1 calc R U . . .
H23B H 0.344687 0.179947 0.475072 0.107 Uiso 1 1 calc R U . . .
H23C H 0.383515 0.174509 0.442778 0.107 Uiso 1 1 calc R U . . .
C24 C 0.23426(9) 0.10942(17) 0.44250(5) 0.0575(4) Uani 1 1 d . . . . .
H24A H 0.196018 0.113667 0.424585 0.086 Uiso 1 1 calc R U . . .
H24B H 0.229912 0.153417 0.463288 0.086 Uiso 1 1 calc R U . . .
H24C H 0.241559 0.035939 0.450263 0.086 Uiso 1 1 calc R U . . .
C25 C 0.34391(5) 0.52229(9) 0.37122(3) 0.0247(2) Uani 1 1 d . . . . .
C26 C 0.35531(6) 0.59379(9) 0.34494(4) 0.0299(3) Uani 1 1 d . . . . .
C27 C 0.38547(6) 0.68794(10) 0.35651(4) 0.0368(3) Uani 1 1 d . . . . .
H27 H 0.394236 0.737700 0.339217 0.044 Uiso 1 1 calc R U . . .
C28 C 0.40279(7) 0.71010(11) 0.39262(4) 0.0420(3) Uani 1 1 d . . . . .
H28 H 0.423561 0.774442 0.400001 0.050 Uiso 1 1 calc R U . . .
C29 C 0.38997(7) 0.63896(12) 0.41800(4) 0.0400(3) Uani 1 1 d . . . . .
H29 H 0.401738 0.655362 0.442805 0.048 Uiso 1 1 calc R U . . .
C30 C 0.36006(6) 0.54325(10) 0.40803(3) 0.0304(3) Uani 1 1 d . . . . .
C31 C 0.33701(7) 0.57136(11) 0.30505(4) 0.0384(3) Uani 1 1 d . . . . .
H31 H 0.313536 0.503144 0.302146 0.046 Uiso 1 1 calc R U . . .
C32 C 0.29463(9) 0.65780(17) 0.28662(5) 0.0597(5) Uani 1 1 d . . . . .
H32A H 0.316958 0.725321 0.288984 0.090 Uiso 1 1 calc R U . . .
H32B H 0.257484 0.663228 0.297914 0.090 Uiso 1 1 calc R U . . .
H32C H 0.282149 0.640548 0.261082 0.090 Uiso 1 1 calc R U . . .
C33 C 0.39417(10) 0.5602(2) 0.28701(5) 0.0694(6) Uani 1 1 d . . . . .
H33A H 0.380868 0.545109 0.261375 0.104 Uiso 1 1 calc R U . . .
H33B H 0.420279 0.502202 0.298283 0.104 Uiso 1 1 calc R U . . .
H33C H 0.418089 0.626127 0.289799 0.104 Uiso 1 1 calc R U . . .
C34 C 0.34710(7) 0.46743(12) 0.43699(4) 0.0372(3) Uani 1 1 d . . . . .
H34 H 0.322892 0.406528 0.424829 0.045 Uiso 1 1 calc R U . . .
C35 C 0.40767(8) 0.42414(14) 0.45841(4) 0.0473(4) Uani 1 1 d . . . . .
H35A H 0.431013 0.387377 0.442130 0.071 Uiso 1 1 calc R U . . .
H35B H 0.398124 0.374655 0.476674 0.071 Uiso 1 1 calc R U . . .
H35C H 0.432779 0.482586 0.470178 0.071 Uiso 1 1 calc R U . . .
C36 C 0.30746(9) 0.51950(16) 0.46208(5) 0.0551(4) Uani 1 1 d . . . . .
H36A H 0.332139 0.573769 0.476611 0.083 Uiso 1 1 calc R U . . .
H36B H 0.294356 0.465856 0.477952 0.083 Uiso 1 1 calc R U . . .
H36C H 0.270588 0.552099 0.447692 0.083 Uiso 1 1 calc R U . . .
C37 C 0.57789(5) 0.08021(9) 0.40838(3) 0.0272(3) Uani 1 1 d . . . . .
C38 C 0.55971(6) -0.00632(10) 0.38608(4) 0.0314(3) Uani 1 1 d . . . . .
C39 C 0.54328(7) -0.09818(10) 0.40246(4) 0.0373(3) Uani 1 1 d . . . . .
H39 H 0.531432 -0.159047 0.388197 0.045 Uiso 1 1 calc R U . . .
C40 C 0.54390(7) -0.10229(11) 0.43892(4) 0.0420(3) Uani 1 1 d . . . . .
H40 H 0.532928 -0.166030 0.449562 0.050 Uiso 1 1 calc R U . . .
C41 C 0.56033(7) -0.01464(12) 0.46022(4) 0.0399(3) Uani 1 1 d . . . . .
H41 H 0.559531 -0.018172 0.485283 0.048 Uiso 1 1 calc R U . . .
C42 C 0.57810(6) 0.07914(10) 0.44533(4) 0.0325(3) Uani 1 1 d . . . . .
C43 C 0.55756(8) -0.00091(12) 0.34582(4) 0.0422(3) Uani 1 1 d . . . . .
H43 H 0.556012 0.075255 0.338705 0.051 Uiso 1 1 calc R U . . .
C44 C 0.49962(9) -0.05486(17) 0.32510(5) 0.0612(5) Uani 1 1 d . . . . .
H44A H 0.503099 -0.131411 0.328739 0.092 Uiso 1 1 calc R U . . .
H44B H 0.495990 -0.038920 0.299415 0.092 Uiso 1 1 calc R U . . .
H44C H 0.462578 -0.028855 0.333850 0.092 Uiso 1 1 calc R U . . .
C45 C 0.61651(9) -0.04934(17) 0.33536(5) 0.0584(5) Uani 1 1 d . . . . .
H45A H 0.653236 -0.011039 0.347559 0.088 Uiso 1 1 calc R U . . .
H45B H 0.614317 -0.044119 0.309268 0.088 Uiso 1 1 calc R U . . .
H45C H 0.619619 -0.123764 0.342583 0.088 Uiso 1 1 calc R U . . .
C46 C 0.59540(7) 0.17595(12) 0.46861(4) 0.0406(3) Uani 1 1 d D U . . .
H46 H 0.615313 0.228504 0.454374 0.049 Uiso 0.581(13) 1 calc R U P B 1
H46A H 0.596711 0.236838 0.451881 0.049 Uiso 0.419(13) 1 calc R U P B 2
C47A C 0.5374(2) 0.2274(5) 0.47946(16) 0.0459(11) Uani 0.581(13) 1 d D U P B 1
H47A H 0.507367 0.244799 0.457795 0.069 Uiso 0.581(13) 1 calc R U P B 1
H47B H 0.549553 0.292100 0.493142 0.069 Uiso 0.581(13) 1 calc R U P B 1
H47C H 0.518223 0.178124 0.494363 0.069 Uiso 0.581(13) 1 calc R U P B 1
C47B C 0.5457(4) 0.1994(9) 0.4897(3) 0.0584(18) Uani 0.419(13) 1 d D U P B 2
H47D H 0.504876 0.192366 0.474249 0.088 Uiso 0.419(13) 1 calc R U P B 2
H47E H 0.550713 0.271725 0.499049 0.088 Uiso 0.419(13) 1 calc R U P B 2
H47F H 0.548521 0.149714 0.509846 0.088 Uiso 0.419(13) 1 calc R U P B 2
C48A C 0.6425(4) 0.1505(5) 0.5041(2) 0.0702(18) Uani 0.581(13) 1 d D U P B 1
H48A H 0.621037 0.110960 0.520668 0.105 Uiso 0.581(13) 1 calc R U P B 1
H48B H 0.658802 0.216705 0.515559 0.105 Uiso 0.581(13) 1 calc R U P B 1
H48C H 0.677079 0.108172 0.498284 0.105 Uiso 0.581(13) 1 calc R U P B 1
C48B C 0.6598(3) 0.1632(6) 0.4893(3) 0.0626(17) Uani 0.419(13) 1 d D U P B 2
H48D H 0.661622 0.099812 0.504416 0.094 Uiso 0.419(13) 1 calc R U P B 2
H48E H 0.670773 0.225246 0.504631 0.094 Uiso 0.419(13) 1 calc R U P B 2
H48F H 0.689296 0.156001 0.472598 0.094 Uiso 0.419(13) 1 calc R U P B 2
C49 C 0.59639(5) 0.43507(9) 0.35631(3) 0.0259(2) Uani 1 1 d . . . . .
C50 C 0.57892(6) 0.43348(11) 0.31890(4) 0.0330(3) Uani 1 1 d . . . . .
C51 C 0.56594(7) 0.52998(12) 0.30149(4) 0.0375(3) Uani 1 1 d . . . . .
H51 H 0.554133 0.531572 0.276067 0.045 Uiso 1 1 calc R U . . .
C52 C 0.56997(6) 0.62313(11) 0.32062(4) 0.0360(3) Uani 1 1 d . . . . .
H52 H 0.560427 0.688163 0.308346 0.043 Uiso 1 1 calc R U . . .
C53 C 0.58782(6) 0.62247(10) 0.35757(4) 0.0317(3) Uani 1 1 d . . . . .
H53 H 0.590683 0.687374 0.370375 0.038 Uiso 1 1 calc R U . . .
C54 C 0.60171(5) 0.52832(10) 0.37639(3) 0.0272(2) Uani 1 1 d D . . . .
C55 C 0.57291(9) 0.33134(13) 0.29740(4) 0.0497(4) Uani 1 1 d . . . . .
H55 H 0.588348 0.271811 0.313975 0.060 Uiso 1 1 calc R U . . .
C56 C 0.50625(11) 0.30858(16) 0.28030(5) 0.0666(5) Uani 1 1 d . . . . .
H56A H 0.480221 0.305137 0.299011 0.100 Uiso 1 1 calc R U . . .
H56B H 0.504311 0.240890 0.267556 0.100 Uiso 1 1 calc R U . . .
H56C H 0.491026 0.364953 0.263241 0.100 Uiso 1 1 calc R U . . .
C57 C 0.61280(12) 0.3362(2) 0.26736(7) 0.0864(8) Uani 1 1 d . . . . .
H57A H 0.597558 0.393241 0.250576 0.130 Uiso 1 1 calc R U . . .
H57B H 0.609789 0.268794 0.254423 0.130 Uiso 1 1 calc R U . . .
H57C H 0.656359 0.349711 0.278021 0.130 Uiso 1 1 calc R U . . .
C58A C 0.62090(8) 0.52763(13) 0.41724(4) 0.0321(4) Uani 0.922(3) 1 d D U P C 1
H58A H 0.650241 0.467077 0.423491 0.039 Uiso 0.922(3) 1 calc R U P C 1
C58B C 0.6012(8) 0.5161(17) 0.4165(3) 0.040(2) Uani 0.078(3) 1 d D U P C 2
H58B H 0.588852 0.442011 0.421176 0.048 Uiso 0.078(3) 1 calc R U P C 2
C59A C 0.65497(8) 0.62717(14) 0.43237(4) 0.0426(4) Uani 0.922(3) 1 d D U P C 1
H59A H 0.689707 0.641159 0.419636 0.064 Uiso 0.922(3) 1 calc R U P C 1
H59B H 0.671049 0.617302 0.458047 0.064 Uiso 0.922(3) 1 calc R U P C 1
H59C H 0.626088 0.687117 0.429171 0.064 Uiso 0.922(3) 1 calc R U P C 1
C59B C 0.6697(7) 0.5300(18) 0.4314(6) 0.050(3) Uani 0.078(3) 1 d D U P C 2
H59D H 0.693702 0.474757 0.421743 0.075 Uiso 0.078(3) 1 calc R U P C 2
H59E H 0.676344 0.524637 0.457707 0.075 Uiso 0.078(3) 1 calc R U P C 2
H59F H 0.683543 0.599480 0.424499 0.075 Uiso 0.078(3) 1 calc R U P C 2
C60A C 0.56452(9) 0.50713(18) 0.43531(5) 0.0536(5) Uani 0.922(3) 1 d D U P C 1
H60A H 0.533767 0.563433 0.428842 0.080 Uiso 0.922(3) 1 calc R U P C 1
H60B H 0.577748 0.505806 0.461474 0.080 Uiso 0.922(3) 1 calc R U P C 1
H60C H 0.545845 0.438981 0.427219 0.080 Uiso 0.922(3) 1 calc R U P C 1
C60B C 0.5582(8) 0.5912(17) 0.4315(5) 0.041(3) Uani 0.078(3) 1 d D U P C 2
H60D H 0.571900 0.664020 0.428820 0.061 Uiso 0.078(3) 1 calc R U P C 2
H60E H 0.559205 0.575746 0.457037 0.061 Uiso 0.078(3) 1 calc R U P C 2
H60F H 0.515590 0.582423 0.418385 0.061 Uiso 0.078(3) 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.2140(15) . ?
O2 C8 1.2160(15) . ?
N1 C2 1.3756(14) . ?
N1 C5 1.3904(14) . ?
N1 C13 1.4386(14) . ?
N2 C2 1.3825(14) . ?
N2 C4 1.3924(15) . ?
N2 C25 1.4453(14) . ?
N3 C10 1.3752(15) . ?
N3 C11 1.3927(16) . ?
N3 C37 1.4401(15) . ?
N4 C10 1.3824(15) . ?
N4 C12 1.3960(16) . ?
N4 C49 1.4375(15) . ?
C2 C6 1.3822(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.3330(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.4859(15) . ?
C6 C8 1.4747(15) . ?
C7 C9 1.4866(15) . ?
C8 C9 1.4803(15) . ?
C9 C10 1.3828(16) . ?
C11 H11 0.9500 . ?
C11 C12 1.330(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.3965(18) . ?
C13 C18 1.3971(18) . ?
C14 C15 1.3935(18) . ?
C14 C19 1.513(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.378(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.3940(19) . ?
C18 C22 1.517(2) . ?
C19 H19 1.0000 . ?
C19 H19A 1.0000 . ?
C19 C20A 1.518(3) . ?
C19 C20B 1.560(6) . ?
C19 C21A 1.556(3) . ?
C19 C21B 1.504(6) . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.525(2) . ?
C22 C24 1.526(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.3966(18) . ?
C25 C30 1.3984(17) . ?
C26 C27 1.3944(18) . ?
C26 C31 1.5164(19) . ?
C27 H27 0.9500 . ?
C27 C28 1.379(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.378(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.3966(19) . ?
C30 C34 1.5173(19) . ?
C31 H31 1.0000 . ?
C31 C32 1.521(2) . ?
C31 C33 1.525(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34 1.0000 . ?
C34 C35 1.526(2) . ?
C34 C36 1.536(2) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.3967(18) . ?
C37 C42 1.3938(19) . ?
C38 C39 1.3925(19) . ?
C38 C43 1.514(2) . ?
C39 H39 0.9500 . ?
C39 C40 1.375(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.381(2) . ?
C41 H41 0.9500 . ?
C41 C42 1.3967(19) . ?
C42 C46 1.5174(19) . ?
C43 H43 1.0000 . ?
C43 C44 1.527(2) . ?
C43 C45 1.535(2) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46 1.0000 . ?
C46 H46A 1.0000 . ?
C46 C47A 1.539(5) . ?
C46 C47B 1.481(7) . ?
C46 C48A 1.575(5) . ?
C46 C48B 1.493(6) . ?
C47A H47A 0.9800 . ?
C47A H47B 0.9800 . ?
C47A H47C 0.9800 . ?
C47B H47D 0.9800 . ?
C47B H47E 0.9800 . ?
C47B H47F 0.9800 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C49 C50 1.3978(18) . ?
C49 C54 1.3969(17) . ?
C50 C51 1.3929(19) . ?
C50 C55 1.520(2) . ?
C51 H51 0.9500 . ?
C51 C52 1.378(2) . ?
C52 H52 0.9500 . ?
C52 C53 1.382(2) . ?
C53 H53 0.9500 . ?
C53 C54 1.3940(17) . ?
C54 C58A 1.5265(19) . ?
C54 C58B 1.522(10) . ?
C55 H55 1.0000 . ?
C55 C56 1.512(3) . ?
C55 C57 1.544(3) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58A H58A 1.0000 . ?
C58A C59A 1.523(2) . ?
C58A C60A 1.526(2) . ?
C58B H58B 1.0000 . ?
C58B C59B 1.513(8) . ?
C58B C60B 1.512(8) . ?
C59A H59A 0.9800 . ?
C59A H59B 0.9800 . ?
C59A H59C 0.9800 . ?
C59B H59D 0.9800 . ?
C59B H59E 0.9800 . ?
C59B H59F 0.9800 . ?
C60A H60A 0.9800 . ?
C60A H60B 0.9800 . ?
C60A H60C 0.9800 . ?
C60B H60D 0.9800 . ?
C60B H60E 0.9800 . ?
C60B H60F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C5 109.85(9) . . ?
C2 N1 C13 126.96(9) . . ?
C5 N1 C13 123.19(10) . . ?
C2 N2 C4 109.54(9) . . ?
C2 N2 C25 125.77(9) . . ?
C4 N2 C25 123.17(9) . . ?
C10 N3 C11 109.70(10) . . ?
C10 N3 C37 127.27(10) . . ?
C11 N3 C37 122.25(10) . . ?
C10 N4 C12 109.61(10) . . ?
C10 N4 C49 125.92(10) . . ?
C12 N4 C49 123.19(10) . . ?
N1 C2 N2 104.88(9) . . ?
N1 C2 C6 128.11(10) . . ?
C6 C2 N2 126.99(10) . . ?
N2 C4 H4 126.1 . . ?
C5 C4 N2 107.85(10) . . ?
C5 C4 H4 126.1 . . ?
N1 C5 H5 126.1 . . ?
C4 C5 N1 107.87(10) . . ?
C4 C5 H5 126.1 . . ?
C2 C6 C7 137.91(10) . . ?
C2 C6 C8 132.73(10) . . ?
C8 C6 C7 89.25(9) . . ?
O1 C7 C6 134.94(11) . . ?
O1 C7 C9 134.54(11) . . ?
C6 C7 C9 90.52(9) . . ?
O2 C8 C6 133.98(11) . . ?
O2 C8 C9 134.81(11) . . ?
C6 C8 C9 91.21(9) . . ?
C8 C9 C7 89.01(9) . . ?
C10 C9 C7 136.78(11) . . ?
C10 C9 C8 134.11(11) . . ?
N3 C10 N4 104.90(10) . . ?
N3 C10 C9 128.08(11) . . ?
N4 C10 C9 127.02(11) . . ?
N3 C11 H11 125.9 . . ?
C12 C11 N3 108.14(11) . . ?
C12 C11 H11 125.9 . . ?
N4 C12 H12 126.2 . . ?
C11 C12 N4 107.64(11) . . ?
C11 C12 H12 126.2 . . ?
C14 C13 N1 118.39(11) . . ?
C14 C13 C18 123.10(12) . . ?
C18 C13 N1 118.46(11) . . ?
C13 C14 C19 121.91(12) . . ?
C15 C14 C13 117.34(13) . . ?
C15 C14 C19 120.75(13) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 120.91(15) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.45(13) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.4 . . ?
C16 C17 C18 121.22(14) . . ?
C18 C17 H17 119.4 . . ?
C13 C18 C22 122.46(12) . . ?
C17 C18 C13 116.97(13) . . ?
C17 C18 C22 120.57(13) . . ?
C14 C19 H19 107.8 . . ?
C14 C19 H19A 108.8 . . ?
C14 C19 C20A 114.3(2) . . ?
C14 C19 C20B 105.3(4) . . ?
C14 C19 C21A 109.42(19) . . ?
C20A C19 H19 107.8 . . ?
C20A C19 C21A 109.4(2) . . ?
C20B C19 H19A 108.8 . . ?
C21A C19 H19 107.8 . . ?
C21B C19 C14 113.8(4) . . ?
C21B C19 H19A 108.8 . . ?
C21B C19 C20B 111.4(5) . . ?
C19 C20A H20A 109.5 . . ?
C19 C20A H20B 109.5 . . ?
C19 C20A H20C 109.5 . . ?
H20A C20A H20B 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C19 C20B H20D 109.5 . . ?
C19 C20B H20E 109.5 . . ?
C19 C20B H20F 109.5 . . ?
H20D C20B H20E 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C19 C21A H21A 109.5 . . ?
C19 C21A H21B 109.5 . . ?
C19 C21A H21C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C19 C21B H21D 109.5 . . ?
C19 C21B H21E 109.5 . . ?
C19 C21B H21F 109.5 . . ?
H21D C21B H21E 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
C18 C22 H22 107.7 . . ?
C18 C22 C23 110.74(15) . . ?
C18 C22 C24 111.91(13) . . ?
C23 C22 H22 107.7 . . ?
C23 C22 C24 110.84(14) . . ?
C24 C22 H22 107.7 . . ?
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 . . ?
C26 C25 N2 119.01(11) . . ?
C26 C25 C30 122.52(11) . . ?
C30 C25 N2 118.46(11) . . ?
C25 C26 C31 122.37(11) . . ?
C27 C26 C25 117.60(12) . . ?
C27 C26 C31 120.03(12) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 C26 121.18(13) . . ?
C28 C27 H27 119.4 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 C27 120.02(13) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 119.3 . . ?
C28 C29 C30 121.38(13) . . ?
C30 C29 H29 119.3 . . ?
C25 C30 C34 123.33(11) . . ?
C29 C30 C25 117.28(13) . . ?
C29 C30 C34 119.39(12) . . ?
C26 C31 H31 108.2 . . ?
C26 C31 C32 110.76(13) . . ?
C26 C31 C33 111.40(13) . . ?
C32 C31 H31 108.2 . . ?
C32 C31 C33 109.91(14) . . ?
C33 C31 H31 108.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 H34 107.8 . . ?
C30 C34 C35 110.95(12) . . ?
C30 C34 C36 111.52(13) . . ?
C35 C34 H34 107.8 . . ?
C35 C34 C36 110.76(12) . . ?
C36 C34 H34 107.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N3 118.62(12) . . ?
C42 C37 N3 118.18(11) . . ?
C42 C37 C38 123.17(12) . . ?
C37 C38 C43 121.74(12) . . ?
C39 C38 C37 117.09(13) . . ?
C39 C38 C43 121.17(13) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.14(13) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.61(13) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 H41 119.6 . . ?
C40 C41 C42 120.72(14) . . ?
C42 C41 H41 119.6 . . ?
C37 C42 C41 117.23(12) . . ?
C37 C42 C46 121.96(12) . . ?
C41 C42 C46 120.80(13) . . ?
C38 C43 H43 107.9 . . ?
C38 C43 C44 111.96(14) . . ?
C38 C43 C45 110.94(13) . . ?
C44 C43 H43 107.9 . . ?
C44 C43 C45 110.14(14) . . ?
C45 C43 H43 107.9 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46 108.3 . . ?
C42 C46 H46A 106.7 . . ?
C42 C46 C47A 111.3(2) . . ?
C42 C46 C48A 112.9(2) . . ?
C47A C46 H46 108.3 . . ?
C47A C46 C48A 107.8(3) . . ?
C47B C46 C42 110.0(4) . . ?
C47B C46 H46A 106.7 . . ?
C47B C46 C48B 116.6(4) . . ?
C48A C46 H46 108.3 . . ?
C48B C46 C42 109.5(3) . . ?
C48B C46 H46A 106.7 . . ?
C46 C47A H47A 109.5 . . ?
C46 C47A H47B 109.5 . . ?
C46 C47A H47C 109.5 . . ?
H47A C47A H47B 109.5 . . ?
H47A C47A H47C 109.5 . . ?
H47B C47A H47C 109.5 . . ?
C46 C47B H47D 109.5 . . ?
C46 C47B H47E 109.5 . . ?
C46 C47B H47F 109.5 . . ?
H47D C47B H47E 109.5 . . ?
H47D C47B H47F 109.5 . . ?
H47E C47B H47F 109.5 . . ?
C46 C48A H48A 109.5 . . ?
C46 C48A H48B 109.5 . . ?
C46 C48A H48C 109.5 . . ?
H48A C48A H48B 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C46 C48B H48D 109.5 . . ?
C46 C48B H48E 109.5 . . ?
C46 C48B H48F 109.5 . . ?
H48D C48B H48E 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C50 C49 N4 118.31(11) . . ?
C54 C49 N4 118.81(11) . . ?
C54 C49 C50 122.89(11) . . ?
C49 C50 C55 122.34(12) . . ?
C51 C50 C49 117.50(12) . . ?
C51 C50 C55 120.16(13) . . ?
C50 C51 H51 119.5 . . ?
C52 C51 C50 120.94(13) . . ?
C52 C51 H51 119.5 . . ?
C51 C52 H52 119.8 . . ?
C51 C52 C53 120.34(12) . . ?
C53 C52 H52 119.8 . . ?
C52 C53 H53 119.4 . . ?
C52 C53 C54 121.22(12) . . ?
C54 C53 H53 119.4 . . ?
C49 C54 C58A 121.73(12) . . ?
C49 C54 C58B 116.0(8) . . ?
C53 C54 C49 117.10(12) . . ?
C53 C54 C58A 121.16(12) . . ?
C53 C54 C58B 123.7(8) . . ?
C50 C55 H55 108.6 . . ?
C50 C55 C57 110.51(16) . . ?
C56 C55 C50 112.22(14) . . ?
C56 C55 H55 108.6 . . ?
C56 C55 C57 108.35(16) . . ?
C57 C55 H55 108.6 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C54 C58A H58A 107.2 . . ?
C59A C58A C54 113.89(13) . . ?
C59A C58A H58A 107.2 . . ?
C59A C58A C60A 110.55(14) . . ?
C60A C58A C54 110.53(13) . . ?
C60A C58A H58A 107.2 . . ?
C54 C58B H58B 108.7 . . ?
C59B C58B C54 100.5(12) . . ?
C59B C58B H58B 108.7 . . ?
C60B C58B C54 114.9(12) . . ?
C60B C58B H58B 108.7 . . ?
C60B C58B C59B 115.0(13) . . ?
C58A C59A H59A 109.5 . . ?
C58A C59A H59B 109.5 . . ?
C58A C59A H59C 109.5 . . ?
H59A C59A H59B 109.5 . . ?
H59A C59A H59C 109.5 . . ?
H59B C59A H59C 109.5 . . ?
C58B C59B H59D 109.5 . . ?
C58B C59B H59E 109.5 . . ?
C58B C59B H59F 109.5 . . ?
H59D C59B H59E 109.5 . . ?
H59D C59B H59F 109.5 . . ?
H59E C59B H59F 109.5 . . ?
C58A C60A H60A 109.5 . . ?
C58A C60A H60B 109.5 . . ?
C58A C60A H60C 109.5 . . ?
H60A C60A H60B 109.5 . . ?
H60A C60A H60C 109.5 . . ?
H60B C60A H60C 109.5 . . ?
C58B C60B H60D 109.5 . . ?
C58B C60B H60E 109.5 . . ?
C58B C60B H60F 109.5 . . ?
H60D C60B H60E 109.5 . . ?
H60D C60B H60F 109.5 . . ?
H60E C60B H60F 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
O1 C7 C9 C8 178.29(17) . . . . ?
O1 C7 C9 C10 1.8(3) . . . . ?
O2 C8 C9 C7 -177.95(16) . . . . ?
O2 C8 C9 C10 -1.3(3) . . . . ?
N1 C2 C6 C7 -9.7(2) . . . . ?
N1 C2 C6 C8 165.39(12) . . . . ?
N1 C13 C14 C15 -178.03(12) . . . . ?
N1 C13 C14 C19 1.87(18) . . . . ?
N1 C13 C18 C17 178.88(11) . . . . ?
N1 C13 C18 C22 -1.12(17) . . . . ?
N2 C2 C6 C7 172.36(12) . . . . ?
N2 C2 C6 C8 -12.6(2) . . . . ?
N2 C4 C5 N1 0.23(14) . . . . ?
N2 C25 C26 C27 -178.80(11) . . . . ?
N2 C25 C26 C31 0.27(18) . . . . ?
N2 C25 C30 C29 178.98(11) . . . . ?
N2 C25 C30 C34 -0.55(18) . . . . ?
N3 C11 C12 N4 0.59(18) . . . . ?
N3 C37 C38 C39 175.40(11) . . . . ?
N3 C37 C38 C43 -4.88(18) . . . . ?
N3 C37 C42 C41 -176.28(11) . . . . ?
N3 C37 C42 C46 5.07(18) . . . . ?
N4 C49 C50 C51 179.54(11) . . . . ?
N4 C49 C50 C55 0.53(19) . . . . ?
N4 C49 C54 C53 -179.20(10) . . . . ?
N4 C49 C54 C58A -0.12(17) . . . . ?
N4 C49 C54 C58B -18.4(7) . . . . ?
C2 N1 C5 C4 -0.88(14) . . . . ?
C2 N1 C13 C14 -89.71(14) . . . . ?
C2 N1 C13 C18 92.61(14) . . . . ?
C2 N2 C4 C5 0.49(13) . . . . ?
C2 N2 C25 C26 109.59(13) . . . . ?
C2 N2 C25 C30 -70.91(15) . . . . ?
C2 C6 C7 O1 -1.9(3) . . . . ?
C2 C6 C7 C9 177.34(14) . . . . ?
C2 C6 C8 O2 1.3(2) . . . . ?
C2 C6 C8 C9 -177.66(13) . . . . ?
C4 N2 C2 N1 -1.00(12) . . . . ?
C4 N2 C2 C6 177.34(11) . . . . ?
C4 N2 C25 C26 -85.92(14) . . . . ?
C4 N2 C25 C30 93.59(14) . . . . ?
C5 N1 C2 N2 1.15(12) . . . . ?
C5 N1 C2 C6 -177.17(11) . . . . ?
C5 N1 C13 C14 89.59(14) . . . . ?
C5 N1 C13 C18 -88.09(14) . . . . ?
C6 C7 C9 C8 -0.96(9) . . . . ?
C6 C7 C9 C10 -177.44(14) . . . . ?
C6 C8 C9 C7 0.97(9) . . . . ?
C6 C8 C9 C10 177.61(13) . . . . ?
C7 C6 C8 O2 177.96(16) . . . . ?
C7 C6 C8 C9 -0.97(9) . . . . ?
C7 C9 C10 N3 -10.5(2) . . . . ?
C7 C9 C10 N4 169.58(13) . . . . ?
C8 C6 C7 O1 -178.28(17) . . . . ?
C8 C6 C7 C9 0.97(9) . . . . ?
C8 C9 C10 N3 174.44(12) . . . . ?
C8 C9 C10 N4 -5.5(2) . . . . ?
C10 N3 C11 C12 -0.23(17) . . . . ?
C10 N3 C37 C38 97.17(15) . . . . ?
C10 N3 C37 C42 -85.06(16) . . . . ?
C10 N4 C12 C11 -0.75(17) . . . . ?
C10 N4 C49 C50 -75.61(16) . . . . ?
C10 N4 C49 C54 104.51(14) . . . . ?
C11 N3 C10 N4 -0.23(14) . . . . ?
C11 N3 C10 C9 179.81(13) . . . . ?
C11 N3 C37 C38 -94.00(16) . . . . ?
C11 N3 C37 C42 83.77(16) . . . . ?
C12 N4 C10 N3 0.59(14) . . . . ?
C12 N4 C10 C9 -179.44(12) . . . . ?
C12 N4 C49 C50 90.10(16) . . . . ?
C12 N4 C49 C54 -89.79(15) . . . . ?
C13 N1 C2 N2 -179.47(10) . . . . ?
C13 N1 C2 C6 2.21(19) . . . . ?
C13 N1 C5 C4 179.71(11) . . . . ?
C13 C14 C15 C16 -0.3(2) . . . . ?
C13 C14 C19 C20A -130.8(3) . . . . ?
C13 C14 C19 C20B -106.7(5) . . . . ?
C13 C14 C19 C21A 106.0(3) . . . . ?
C13 C14 C19 C21B 131.0(7) . . . . ?
C13 C18 C22 C23 -109.60(16) . . . . ?
C13 C18 C22 C24 126.20(14) . . . . ?
C14 C13 C18 C17 1.31(18) . . . . ?
C14 C13 C18 C22 -178.69(12) . . . . ?
C14 C15 C16 C17 0.1(2) . . . . ?
C15 C14 C19 C20A 49.1(3) . . . . ?
C15 C14 C19 C20B 73.1(5) . . . . ?
C15 C14 C19 C21A -74.1(3) . . . . ?
C15 C14 C19 C21B -49.1(7) . . . . ?
C15 C16 C17 C18 0.8(2) . . . . ?
C16 C17 C18 C13 -1.47(19) . . . . ?
C16 C17 C18 C22 178.53(13) . . . . ?
C17 C18 C22 C23 70.40(18) . . . . ?
C17 C18 C22 C24 -53.81(19) . . . . ?
C18 C13 C14 C15 -0.46(19) . . . . ?
C18 C13 C14 C19 179.43(12) . . . . ?
C19 C14 C15 C16 179.83(14) . . . . ?
C25 N2 C2 N1 165.27(10) . . . . ?
C25 N2 C2 C6 -16.39(18) . . . . ?
C25 N2 C4 C5 -166.20(11) . . . . ?
C25 C26 C27 C28 -0.7(2) . . . . ?
C25 C26 C31 C32 123.28(15) . . . . ?
C25 C26 C31 C33 -114.04(16) . . . . ?
C25 C30 C34 C35 113.27(14) . . . . ?
C25 C30 C34 C36 -122.75(14) . . . . ?
C26 C25 C30 C29 -1.53(18) . . . . ?
C26 C25 C30 C34 178.94(12) . . . . ?
C26 C27 C28 C29 -0.4(2) . . . . ?
C27 C26 C31 C32 -57.66(18) . . . . ?
C27 C26 C31 C33 65.01(18) . . . . ?
C27 C28 C29 C30 0.6(2) . . . . ?
C28 C29 C30 C25 0.3(2) . . . . ?
C28 C29 C30 C34 179.88(13) . . . . ?
C29 C30 C34 C35 -66.25(16) . . . . ?
C29 C30 C34 C36 57.73(18) . . . . ?
C30 C25 C26 C27 1.71(18) . . . . ?
C30 C25 C26 C31 -179.21(12) . . . . ?
C31 C26 C27 C28 -179.79(13) . . . . ?
C37 N3 C10 N4 169.75(12) . . . . ?
C37 N3 C10 C9 -10.2(2) . . . . ?
C37 N3 C11 C12 -170.81(13) . . . . ?
C37 C38 C39 C40 1.2(2) . . . . ?
C37 C38 C43 C44 -138.03(14) . . . . ?
C37 C38 C43 C45 98.49(16) . . . . ?
C37 C42 C46 C47A 105.3(3) . . . . ?
C37 C42 C46 C47B 126.9(5) . . . . ?
C37 C42 C46 C48A -133.4(5) . . . . ?
C37 C42 C46 C48B -103.7(5) . . . . ?
C38 C37 C42 C41 1.38(19) . . . . ?
C38 C37 C42 C46 -177.28(12) . . . . ?
C38 C39 C40 C41 0.7(2) . . . . ?
C39 C38 C43 C44 41.68(19) . . . . ?
C39 C38 C43 C45 -81.81(18) . . . . ?
C39 C40 C41 C42 -1.6(2) . . . . ?
C40 C41 C42 C37 0.6(2) . . . . ?
C40 C41 C42 C46 179.24(13) . . . . ?
C41 C42 C46 C47A -73.3(3) . . . . ?
C41 C42 C46 C47B -51.7(5) . . . . ?
C41 C42 C46 C48A 48.0(5) . . . . ?
C41 C42 C46 C48B 77.7(5) . . . . ?
C42 C37 C38 C39 -2.25(18) . . . . ?
C42 C37 C38 C43 177.47(12) . . . . ?
C43 C38 C39 C40 -178.52(13) . . . . ?
C49 N4 C10 N3 167.93(11) . . . . ?
C49 N4 C10 C9 -12.1(2) . . . . ?
C49 N4 C12 C11 -168.50(13) . . . . ?
C49 C50 C51 C52 -0.3(2) . . . . ?
C49 C50 C55 C56 113.05(16) . . . . ?
C49 C50 C55 C57 -125.90(17) . . . . ?
C49 C54 C58A C59A 150.87(13) . . . . ?
C49 C54 C58A C60A -83.97(18) . . . . ?
C49 C54 C58B C59B 103.4(12) . . . . ?
C49 C54 C58B C60B -132.6(12) . . . . ?
C50 C49 C54 C53 0.92(17) . . . . ?
C50 C49 C54 C58A -179.99(12) . . . . ?
C50 C49 C54 C58B 161.7(7) . . . . ?
C50 C51 C52 C53 0.8(2) . . . . ?
C51 C50 C55 C56 -65.94(19) . . . . ?
C51 C50 C55 C57 55.1(2) . . . . ?
C51 C52 C53 C54 -0.5(2) . . . . ?
C52 C53 C54 C49 -0.39(18) . . . . ?
C52 C53 C54 C58A -179.48(12) . . . . ?
C52 C53 C54 C58B -159.6(8) . . . . ?
C53 C54 C58A C59A -30.08(19) . . . . ?
C53 C54 C58A C60A 95.07(17) . . . . ?
C53 C54 C58B C59B -97.2(12) . . . . ?
C53 C54 C58B C60B 26.8(17) . . . . ?
C54 C49 C50 C51 -0.58(19) . . . . ?
C54 C49 C50 C55 -179.59(13) . . . . ?
C55 C50 C51 C52 178.73(14) . . . . ?

_olex2_date_sample_data_collection 2021-05-06
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.773
####################################################################### 
# 
# 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_wf457
_database_code_depnum_ccdc_archive 'CCDC 2108061'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-09-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-09-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H8 N2 O'
_chemical_formula_sum            'C7 H8 N2 O'
_chemical_formula_weight         136.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C7 H8 N2 O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   6.2198(3)
_cell_length_b                   15.0126(7)
_cell_length_c                   7.3727(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.876(4)
_cell_angle_gamma                90
_cell_volume                     683.47(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2224
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.2230
_cell_measurement_theta_min      5.8670
_shelx_estimated_absorpt_T_max   0.978
_shelx_estimated_absorpt_T_min   0.852
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0110
1 0 0 0.0205
0 1 0 0.0521
0 -1 0 0.1195
0 1 -1 0.0691
0 -1 1 0.1220
0 0 -1 0.1109
0 0 1 0.1050
0 2 1 0.0466
1 -2 -2 0.1270

_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
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
-1.0000 0.0000 0.0000 -0.2090 0.0694 0.1177
1.0000 -0.0000 -0.0000 0.2090 -0.0694 -0.1177
0.0000 1.0000 0.0000 -0.0078 -0.0933 0.0418
-0.0000 -1.0000 -0.0000 0.0078 0.0933 -0.0418
0.0000 1.0001 -1.0000 0.0841 -0.0225 0.2174
-0.0000 -1.0001 1.0000 -0.0841 0.0225 -0.2174
0.0000 0.0001 -1.0000 0.0920 0.0708 0.1756
-0.0000 -0.0001 1.0000 -0.0920 -0.0708 -0.1756
-0.0000 2.0000 1.0000 -0.1076 -0.2574 -0.0921
1.0000 -1.9999 -2.0000 0.4086 0.2588 0.1500

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0119
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3278
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.347
_diffrn_reflns_theta_min         5.895
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  -1.00   1.00    2.00    --  -43.50  91.00 142.00   33
  2  ω     38.00  73.00   1.00    2.00    --   43.55 -91.00  28.00   35
  3  ω    105.00 175.00   1.00   10.00    --  103.26  91.00 142.00   70
  4  ω     64.00  96.00   1.00   10.00    --  103.26 -91.00  28.00   32
  5  ω    -65.00  26.00   1.00    2.00    --  -43.50  37.00  30.00   91
  6  ω     29.00  75.00   1.00    2.00    --   43.55 -99.00 -60.00   46
  7  ω     23.00 112.00   1.00    2.00    --   43.55  37.00-120.00   89
  8  ω     55.00  82.00   1.00   10.00    --  103.26 -45.00  30.00   27
  9  ω    122.00 170.00   1.00   10.00    --  103.26  77.00 -60.00   48
 10  ω     48.00 107.00   1.00   10.00    --  103.26 -94.00 -60.00   59
 11  ω     98.00 169.00   1.00   10.00    --  103.26 125.00-120.00   71
 12  ω    104.00 170.00   1.00   10.00    --  103.26  77.00  30.00   66
 13  ω    103.00 176.00   1.00   10.00    --  103.26  77.00   0.00   73
 14  ω     75.00 100.00   1.00   10.00    --  103.26 -77.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2090385000
_diffrn_orient_matrix_UB_12      -0.0078372000
_diffrn_orient_matrix_UB_13      -0.0919675000
_diffrn_orient_matrix_UB_21      -0.0693664000
_diffrn_orient_matrix_UB_22      -0.0932835000
_diffrn_orient_matrix_UB_23      -0.0708072000
_diffrn_orient_matrix_UB_31      -0.1177039000
_diffrn_orient_matrix_UB_32      0.0417765000
_diffrn_orient_matrix_UB_33      -0.1756281000
_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                1156
_reflns_number_total             1312
_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 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.127
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0321
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0492P)²+0.1051P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0891
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H8D)=Sof(H8E)=Sof(H8F)=1-FVAR(1)
 Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(H9D)=Sof(H9E)=Sof(H9F)=1-FVAR(2)
 Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
3.b Disordered Me refined as rotating group:
 C8(H8A,H8B,H8C,H8D,H8E,H8F), C9(H9A,H9B,H9C,H9D,H9E,H9F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.20145(14) 0.45355(5) 0.19943(12) 0.0401(2) Uani 1 1 d . . . . .
N1 N 0.58020(14) 0.17705(6) 0.37507(11) 0.0259(2) Uani 1 1 d . . . . .
N2 N 0.75737(14) 0.29759(6) 0.45628(11) 0.0266(2) Uani 1 1 d . . . . .
C2 C 0.56593(16) 0.26691(7) 0.37158(13) 0.0248(2) Uani 1 1 d . . . . .
C4 C 0.89002(18) 0.22652(8) 0.51215(14) 0.0300(3) Uani 1 1 d . . . . .
H4 H 1.032692 0.229890 0.574272 0.036 Uiso 1 1 calc R U . . .
C5 C 0.77963(17) 0.15158(8) 0.46226(14) 0.0297(3) Uani 1 1 d . . . . .
H5 H 0.829597 0.092234 0.483133 0.036 Uiso 1 1 calc R U . . .
C6 C 0.38750(18) 0.31548(8) 0.29670(15) 0.0298(3) Uani 1 1 d . . . . .
C7 C 0.30384(17) 0.38826(7) 0.25150(14) 0.0268(3) Uani 1 1 d . . . . .
C8 C 0.40538(18) 0.11771(8) 0.30236(15) 0.0316(3) Uani 1 1 d . . . . .
H8A H 0.279021 0.127683 0.367406 0.038 Uiso 0.837(14) 1 calc R U P . .
H8B H 0.453125 0.055718 0.318821 0.038 Uiso 0.837(14) 1 calc R U P . .
H8C H 0.366447 0.129820 0.171945 0.038 Uiso 0.837(14) 1 calc R U P . .
H8D H 0.453375 0.081131 0.204708 0.038 Uiso 0.163(14) 1 calc R U P . .
H8E H 0.279270 0.153096 0.253294 0.038 Uiso 0.163(14) 1 calc R U P . .
H8F H 0.365948 0.078994 0.400170 0.038 Uiso 0.163(14) 1 calc R U P . .
C9 C 0.81587(19) 0.39118(8) 0.47532(16) 0.0334(3) Uani 1 1 d . . . . .
H9A H 0.878996 0.410919 0.366551 0.040 Uiso 0.680(15) 1 calc R U P . .
H9B H 0.921829 0.399195 0.583618 0.040 Uiso 0.680(15) 1 calc R U P . .
H9C H 0.686194 0.426517 0.488608 0.040 Uiso 0.680(15) 1 calc R U P . .
H9D H 0.779017 0.413502 0.592634 0.040 Uiso 0.320(15) 1 calc R U P . .
H9E H 0.736183 0.425226 0.375567 0.040 Uiso 0.320(15) 1 calc R U P . .
H9F H 0.971819 0.397903 0.470576 0.040 Uiso 0.320(15) 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.2063(14) . ?
N1 C2 1.3519(15) . ?
N1 C5 1.3811(14) . ?
N1 C8 1.4573(14) . ?
N2 C2 1.3572(13) . ?
N2 C4 1.3811(14) . ?
N2 C9 1.4540(14) . ?
C2 C6 1.3861(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.3461(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.2386(16) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 H8D 0.9800 . ?
C8 H8E 0.9800 . ?
C8 H8F 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 H9D 0.9800 . ?
C9 H9E 0.9800 . ?
C9 H9F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C5 109.78(9) . . ?
C2 N1 C8 123.96(9) . . ?
C5 N1 C8 126.22(10) . . ?
C2 N2 C4 109.57(9) . . ?
C2 N2 C9 124.61(9) . . ?
C4 N2 C9 125.74(9) . . ?
N1 C2 N2 106.13(9) . . ?
N1 C2 C6 125.45(10) . . ?
N2 C2 C6 128.41(10) . . ?
N2 C4 H4 126.4 . . ?
C5 C4 N2 107.29(9) . . ?
C5 C4 H4 126.4 . . ?
N1 C5 H5 126.4 . . ?
C4 C5 N1 107.22(10) . . ?
C4 C5 H5 126.4 . . ?
C7 C6 C2 149.51(12) . . ?
O1 C7 C6 172.39(12) . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
N1 C8 H8D 109.5 . . ?
N1 C8 H8E 109.5 . . ?
N1 C8 H8F 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8A C8 H8D 141.1 . . ?
H8A C8 H8E 56.3 . . ?
H8A C8 H8F 56.3 . . ?
H8B C8 H8C 109.5 . . ?
H8B C8 H8D 56.3 . . ?
H8B C8 H8E 141.1 . . ?
H8B C8 H8F 56.3 . . ?
H8C C8 H8D 56.3 . . ?
H8C C8 H8E 56.3 . . ?
H8C C8 H8F 141.1 . . ?
H8D C8 H8E 109.5 . . ?
H8D C8 H8F 109.5 . . ?
H8E C8 H8F 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
N2 C9 H9D 109.5 . . ?
N2 C9 H9E 109.5 . . ?
N2 C9 H9F 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9A C9 H9D 141.1 . . ?
H9A C9 H9E 56.3 . . ?
H9A C9 H9F 56.3 . . ?
H9B C9 H9C 109.5 . . ?
H9B C9 H9D 56.3 . . ?
H9B C9 H9E 141.1 . . ?
H9B C9 H9F 56.3 . . ?
H9C C9 H9D 56.3 . . ?
H9C C9 H9E 56.3 . . ?
H9C C9 H9F 141.1 . . ?
H9D C9 H9E 109.5 . . ?
H9D C9 H9F 109.5 . . ?
H9E C9 H9F 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 C2 C6 C7 -172.76(18) . . . . ?
N2 C2 C6 C7 8.0(3) . . . . ?
N2 C4 C5 N1 0.34(12) . . . . ?
C2 N1 C5 C4 -0.35(12) . . . . ?
C2 N2 C4 C5 -0.21(12) . . . . ?
C4 N2 C2 N1 0.00(11) . . . . ?
C4 N2 C2 C6 179.38(10) . . . . ?
C5 N1 C2 N2 0.22(11) . . . . ?
C5 N1 C2 C6 -179.20(10) . . . . ?
C8 N1 C2 N2 178.18(9) . . . . ?
C8 N1 C2 C6 -1.23(16) . . . . ?
C8 N1 C5 C4 -178.26(10) . . . . ?
C9 N2 C2 N1 176.91(9) . . . . ?
C9 N2 C2 C6 -3.70(17) . . . . ?
C9 N2 C4 C5 -177.08(10) . . . . ?

_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.420
_oxdiff_exptl_absorpt_empirical_full_min 0.705
####################################################################### 
# 
# 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_wf446pd
_database_code_depnum_ccdc_archive 'CCDC 2094755'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-05-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H41 Cl N2 O Pd, C6 H6'
_chemical_formula_sum            'C38 H47 Cl N2 O Pd'
_chemical_formula_weight         689.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H47 Cl N2 O Pd'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.2887(3)
_cell_length_b                   12.5359(4)
_cell_length_c                   16.8607(5)
_cell_angle_alpha                86.331(3)
_cell_angle_beta                 82.998(3)
_cell_angle_gamma                86.923(3)
_cell_volume                     1733.45(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9162
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4520
_cell_measurement_theta_min      3.4680
_shelx_estimated_absorpt_T_max   0.779
_shelx_estimated_absorpt_T_min   0.331
_exptl_absorpt_coefficient_mu    5.254
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 2 0.0273
-1 1 -2 0.0236
-2 -2 1 0.0492
2 2 -1 0.0344
0 -1 0 0.0723
0 1 0 0.0759
-1 0 1 0.1027
-2 1 -5 0.0235
2 0 5 0.0415

_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
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
1.0000 -1.0000 2.0000 -0.2398 -0.0182 0.1520
-1.0000 1.0000 -2.0000 0.2398 0.0182 -0.1520
-2.0000 -2.0000 1.0000 0.0815 -0.4531 -0.0138
2.0000 2.0000 -1.0000 -0.0815 0.4531 0.0138
-0.0000 -1.0000 0.0000 -0.0029 -0.0675 0.1031
0.0000 1.0000 -0.0000 0.0029 0.0675 -0.1031
-1.0000 0.0000 1.0000 0.0050 -0.1810 -0.1223
-2.0000 1.0000 -5.0000 0.5540 0.0128 -0.1763
2.0000 0.0000 5.0000 -0.5511 0.0547 0.0732

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14148
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.576
_diffrn_reflns_theta_min         3.537
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  14.00   1.00    1.00    --  -43.01 104.00 -99.00   96
  2  ω     37.00  64.00   1.00    1.00    --   43.01-104.00 159.00   27
  3  ω     44.00 107.00   1.00    4.00    --  103.80-104.00 159.00   63
  4  ω    111.00 146.00   1.00    4.00    --  103.80 104.00 -99.00   35
  5  ω    -61.00 -25.00   1.00    1.00    --  -43.01 -37.00-180.00   36
  6  ω   -116.00 -73.00   1.00    1.00    --  -43.01 -37.00-180.00   43
  7  ω    -66.00  31.00   1.00    1.00    --  -43.01  37.00-180.00   97
  8  ω     33.00 115.00   1.00    1.00    --   43.01  57.00  30.00   82
  9  ω     29.00  56.00   1.00    1.00    --   43.01 -99.00 -30.00   27
 10  ω     27.00 104.00   1.00    4.00    --  103.80-111.00  90.00   77
 11  ω     24.00 104.00   1.00    4.00    --  103.80 -94.00 -60.00   80
 12  ω     32.00  94.00   1.00    4.00    --  103.80 -61.00 -30.00   62
 13  ω    128.00 172.00   1.00    4.00    --  103.80  45.00 -30.00   44
 14  ω     21.00  64.00   1.00    4.00    --  103.80 -94.00-180.00   43
 15  ω     82.00 107.00   1.00    4.00    --  103.80 -94.00-180.00   25
 16  ω     98.00 177.00   1.00    4.00    --  103.80  45.00 120.00   79
 17  ω     31.00  58.00   1.00    4.00    --  103.80-111.00 -60.00   27
 18  ω     81.00 108.00   1.00    4.00    --  103.80-111.00  60.00   27
 19  ω     27.00  53.00   1.00    4.00    --  103.80-111.00  60.00   26
 20  ω     57.00 129.00   1.00    4.00    --  103.80 -61.00 150.00   72
 21  ω     84.00 111.00   1.00    4.00    --  103.80  45.00 -30.00   27
 22  ω     83.00 108.00   1.00    4.00    --  103.80-111.00 -60.00   25
 23  ω    137.00 170.00   1.00    4.00    --  103.80 111.00-150.00   33
 24  ω     77.00 177.00   1.00    4.00    --  103.80  30.00-120.00  100
 25  ω    132.00 159.00   1.00    4.00    --  103.80  77.00 150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0822906000
_diffrn_orient_matrix_UB_12      0.0028729000
_diffrn_orient_matrix_UB_13      -0.0773001000
_diffrn_orient_matrix_UB_21      0.1371271000
_diffrn_orient_matrix_UB_22      0.0674751000
_diffrn_orient_matrix_UB_23      -0.0439075000
_diffrn_orient_matrix_UB_31      0.0978040000
_diffrn_orient_matrix_UB_32      -0.1031310000
_diffrn_orient_matrix_UB_33      -0.0244906000
_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                6159
_reflns_number_total             6693
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6693
_refine_ls_number_restraints     212
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.098
_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)+(0.0130P)²+0.3649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0685
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9A-C10 \\sim C9B-C10
 with sigma of 0.02
 C9A-C8 \\sim C9B-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C8 \\sim C9A \\sim C9B \\sim C10: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C35A \\sim C35B \\sim C36A \\sim C36B \\sim C37A \\sim C37B \\sim C38A \\sim
C38B \\sim C39A \\sim C39B \\sim C40A \\sim C40B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(C9B)=Sof(H9B)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9A)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C37B)=Sof(H37B)=Sof(C36B)=Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(C40B)=
 Sof(H40B)=Sof(C39B)=Sof(H39B)=Sof(C38B)=Sof(H38B)=1-FVAR(2)
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=
 Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C9A(H9A), C9B(H9B), C17(H17), C20(H20), C29(H29), C32(H32)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8BC,H8BD), C8(H8AA,H8AB), C10(H10C,H10D), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C13(H13), C14(H14), C15(H15), C25(H25), C26(H26), C27(H27),
 C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A),
 C37B(H37B), C36B(H36B), C35B(H35B), C40B(H40B), C39B(H39B), C38B(H38B)
5.d Fitted hexagon refined as free rotating group:
 C37B(C36B,C35B,C40B,C39B,C38B)
5.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.75696(2) 0.19949(2) 0.82124(2) 0.02543(6) Uani 1 1 d . . . . .
Cl1 Cl 0.89553(8) 0.23299(6) 0.69258(4) 0.03991(15) Uani 1 1 d . . . . .
O1 O 0.8004(2) 0.48254(14) 0.86199(12) 0.0380(4) Uani 1 1 d . . . . .
N1 N 0.3812(2) 0.30455(14) 0.75790(11) 0.0208(4) Uani 1 1 d . . . . .
N2 N 0.4551(2) 0.46697(14) 0.73078(11) 0.0198(4) Uani 1 1 d . . . . .
C2 C 0.4950(3) 0.37317(16) 0.77100(13) 0.0190(4) Uani 1 1 d . . . . .
C4 C 0.3169(3) 0.45596(18) 0.69434(13) 0.0233(4) Uani 1 1 d . . . . .
H4 H 0.264120 0.510003 0.663304 0.028 Uiso 1 1 calc R U . . .
C5 C 0.2704(3) 0.35506(18) 0.71070(14) 0.0246(5) Uani 1 1 d . . . . .
H5 H 0.179490 0.324258 0.693335 0.030 Uiso 1 1 calc R U . . .
C6 C 0.6263(3) 0.35140(16) 0.81562(14) 0.0224(4) Uani 1 1 d . . . . .
C7 C 0.7141(3) 0.42467(18) 0.83778(14) 0.0261(5) Uani 1 1 d . . . . .
C8 C 0.8616(4) 0.0415(2) 0.8419(2) 0.0452(7) Uani 1 1 d D U . . .
H8BC H 0.793884 -0.018709 0.833840 0.054 Uiso 0.475(8) 1 calc R U P A 2
H8BD H 0.977927 0.029597 0.821520 0.054 Uiso 0.475(8) 1 calc R U P A 2
H8AA H 0.864926 -0.007272 0.797710 0.054 Uiso 0.525(8) 1 calc R U P A 1
H8AB H 0.961219 0.035886 0.869105 0.054 Uiso 0.525(8) 1 calc R U P A 1
C9A C 0.7192(6) 0.0523(4) 0.8889(3) 0.0402(14) Uani 0.525(8) 1 d D U P A 1
H9A H 0.627509 0.009142 0.877556 0.048 Uiso 0.525(8) 1 calc R U P A 1
C9B C 0.8281(7) 0.0894(4) 0.9141(4) 0.0388(15) Uani 0.475(8) 1 d D U P A 2
H9B H 0.922974 0.107666 0.941161 0.047 Uiso 0.475(8) 1 calc R U P A 2
C10 C 0.6816(4) 0.1379(2) 0.93848(17) 0.0422(6) Uani 1 1 d D U . . .
H10C H 0.679604 0.188122 0.981619 0.051 Uiso 0.475(8) 1 calc R U P A 2
H10D H 0.586660 0.092097 0.944932 0.051 Uiso 0.475(8) 1 calc R U P A 2
H10A H 0.755989 0.146518 0.979064 0.051 Uiso 0.525(8) 1 calc R U P A 1
H10B H 0.565302 0.150640 0.958640 0.051 Uiso 0.525(8) 1 calc R U P A 1
C11 C 0.3617(3) 0.19704(17) 0.79344(14) 0.0225(4) Uani 1 1 d . . . . .
C12 C 0.4022(3) 0.11137(18) 0.74391(15) 0.0255(5) Uani 1 1 d . . . . .
C13 C 0.3710(3) 0.00948(19) 0.77862(16) 0.0329(5) Uani 1 1 d . . . . .
H13 H 0.395856 -0.050835 0.747215 0.039 Uiso 1 1 calc R U . . .
C14 C 0.3052(3) -0.00591(19) 0.85701(17) 0.0329(5) Uani 1 1 d . . . . .
H14 H 0.283774 -0.076216 0.878755 0.039 Uiso 1 1 calc R U . . .
C15 C 0.2699(3) 0.08027(19) 0.90462(16) 0.0297(5) Uani 1 1 d . . . . .
H15 H 0.226605 0.068153 0.959066 0.036 Uiso 1 1 calc R U . . .
C16 C 0.2970(3) 0.18434(18) 0.87398(15) 0.0254(5) Uani 1 1 d . . . . .
C17 C 0.4736(3) 0.12697(19) 0.65696(15) 0.0308(5) Uani 1 1 d . . . . .
H17 H 0.521144 0.199090 0.649431 0.037 Uiso 1 1 calc R U . . .
C18 C 0.3434(4) 0.1248(2) 0.60053(17) 0.0416(6) Uani 1 1 d . . . . .
H18A H 0.297528 0.053939 0.605262 0.062 Uiso 1 1 calc R U . . .
H18B H 0.392214 0.140061 0.545313 0.062 Uiso 1 1 calc R U . . .
H18C H 0.256951 0.179054 0.614752 0.062 Uiso 1 1 calc R U . . .
C19 C 0.6107(3) 0.0434(2) 0.63429(18) 0.0394(6) Uani 1 1 d . . . . .
H19A H 0.692056 0.043291 0.671854 0.059 Uiso 1 1 calc R U . . .
H19B H 0.661939 0.060965 0.579873 0.059 Uiso 1 1 calc R U . . .
H19C H 0.565520 -0.027604 0.636669 0.059 Uiso 1 1 calc R U . . .
C20 C 0.2550(3) 0.27893(19) 0.92630(15) 0.0276(5) Uani 1 1 d . . . . .
H20 H 0.342519 0.331104 0.911905 0.033 Uiso 1 1 calc R U . . .
C21 C 0.0949(3) 0.3363(2) 0.90930(17) 0.0377(6) Uani 1 1 d . . . . .
H21A H 0.099119 0.356007 0.851923 0.057 Uiso 1 1 calc R U . . .
H21B H 0.077314 0.400994 0.939488 0.057 Uiso 1 1 calc R U . . .
H21C H 0.005196 0.288692 0.925577 0.057 Uiso 1 1 calc R U . . .
C22 C 0.2494(4) 0.2499(2) 1.01585(16) 0.0416(6) Uani 1 1 d . . . . .
H22A H 0.153988 0.207847 1.033841 0.062 Uiso 1 1 calc R U . . .
H22B H 0.242187 0.315443 1.045004 0.062 Uiso 1 1 calc R U . . .
H22C H 0.348354 0.207612 1.026222 0.062 Uiso 1 1 calc R U . . .
C23 C 0.5280(3) 0.56655(17) 0.73874(14) 0.0221(4) Uani 1 1 d . . . . .
C24 C 0.6652(3) 0.59423(18) 0.68672(15) 0.0281(5) Uani 1 1 d . . . . .
C25 C 0.7296(3) 0.6925(2) 0.69557(18) 0.0378(6) Uani 1 1 d . . . . .
H25 H 0.821969 0.714635 0.660621 0.045 Uiso 1 1 calc R U . . .
C26 C 0.6607(4) 0.7581(2) 0.75465(19) 0.0404(6) Uani 1 1 d . . . . .
H26 H 0.705970 0.825055 0.759675 0.048 Uiso 1 1 calc R U . . .
C27 C 0.5270(3) 0.72746(19) 0.80639(16) 0.0343(6) Uani 1 1 d . . . . .
H27 H 0.482518 0.773109 0.847193 0.041 Uiso 1 1 calc R U . . .
C28 C 0.4564(3) 0.63089(18) 0.79974(14) 0.0261(5) Uani 1 1 d . . . . .
C29 C 0.7435(3) 0.5209(2) 0.62311(16) 0.0344(6) Uani 1 1 d . . . . .
H29 H 0.700451 0.448054 0.636449 0.041 Uiso 1 1 calc R U . . .
C30 C 0.9277(4) 0.5110(3) 0.6218(2) 0.0477(7) Uani 1 1 d . . . . .
H30A H 0.973865 0.580136 0.604239 0.072 Uiso 1 1 calc R U . . .
H30B H 0.972699 0.456937 0.584716 0.072 Uiso 1 1 calc R U . . .
H30C H 0.955005 0.489627 0.675684 0.072 Uiso 1 1 calc R U . . .
C31 C 0.6969(4) 0.5594(3) 0.54100(19) 0.0558(9) Uani 1 1 d . . . . .
H31A H 0.578274 0.561483 0.542348 0.084 Uiso 1 1 calc R U . . .
H31B H 0.746233 0.510267 0.500999 0.084 Uiso 1 1 calc R U . . .
H31C H 0.736349 0.631286 0.526864 0.084 Uiso 1 1 calc R U . . .
C32 C 0.3106(3) 0.59638(19) 0.85733(15) 0.0329(5) Uani 1 1 d . . . . .
H32 H 0.288029 0.522099 0.844837 0.040 Uiso 1 1 calc R U . . .
C33 C 0.1584(4) 0.6655(3) 0.8469(3) 0.0613(10) Uani 1 1 d . . . . .
H33A H 0.175436 0.739099 0.859360 0.092 Uiso 1 1 calc R U . . .
H33B H 0.066833 0.637547 0.883089 0.092 Uiso 1 1 calc R U . . .
H33C H 0.134460 0.664767 0.791426 0.092 Uiso 1 1 calc R U . . .
C34 C 0.3481(5) 0.5913(4) 0.9432(2) 0.0720(12) Uani 1 1 d . . . . .
H34A H 0.444756 0.544076 0.948573 0.108 Uiso 1 1 calc R U . . .
H34B H 0.255279 0.563240 0.978538 0.108 Uiso 1 1 calc R U . . .
H34C H 0.368431 0.663213 0.958110 0.108 Uiso 1 1 calc R U . . .
C35A C 0.7520(8) 0.2078(5) 0.3606(4) 0.0511(14) Uani 0.685(7) 1 d . U P B 1
H35A H 0.684782 0.222024 0.319008 0.061 Uiso 0.685(7) 1 calc R U P B 1
C36A C 0.8819(8) 0.1378(5) 0.3507(4) 0.0516(14) Uani 0.685(7) 1 d . U P B 1
H36A H 0.905930 0.103406 0.301733 0.062 Uiso 0.685(7) 1 calc R U P B 1
C37A C 0.9799(7) 0.1159(5) 0.4107(4) 0.0508(14) Uani 0.685(7) 1 d . U P B 1
H37A H 1.067963 0.064295 0.404067 0.061 Uiso 0.685(7) 1 calc R U P B 1
C38A C 0.9497(7) 0.1689(5) 0.4801(4) 0.0441(14) Uani 0.685(7) 1 d . U P B 1
H38A H 1.019497 0.156161 0.520752 0.053 Uiso 0.685(7) 1 calc R U P B 1
C39A C 0.8183(8) 0.2403(4) 0.4907(3) 0.0468(13) Uani 0.685(7) 1 d . U P B 1
H39A H 0.796984 0.277119 0.538651 0.056 Uiso 0.685(7) 1 calc R U P B 1
C40A C 0.7176(7) 0.2585(4) 0.4315(4) 0.0478(13) Uani 0.685(7) 1 d . U P B 1
H40A H 0.624500 0.305873 0.439381 0.057 Uiso 0.685(7) 1 calc R U P B 1
C37B C 0.9666(11) 0.1023(6) 0.3693(6) 0.045(2) Uani 0.315(7) 1 d G U P B 2
H37B H 1.031590 0.050386 0.339714 0.054 Uiso 0.315(7) 1 calc R U P B 2
C36B C 0.8351(14) 0.1550(9) 0.3376(5) 0.051(2) Uani 0.315(7) 1 d G U P B 2
H36B H 0.810190 0.139114 0.286186 0.061 Uiso 0.315(7) 1 calc R U P B 2
C35B C 0.7399(11) 0.2311(9) 0.3809(8) 0.052(2) Uani 0.315(7) 1 d G U P B 2
H35B H 0.650056 0.267081 0.359176 0.063 Uiso 0.315(7) 1 calc R U P B 2
C40B C 0.7763(14) 0.2544(7) 0.4561(7) 0.053(2) Uani 0.315(7) 1 d G U P B 2
H40B H 0.711320 0.306322 0.485694 0.063 Uiso 0.315(7) 1 calc R U P B 2
C39B C 0.9078(15) 0.2017(9) 0.4879(5) 0.046(2) Uani 0.315(7) 1 d G U P B 2
H39B H 0.932718 0.217594 0.539223 0.056 Uiso 0.315(7) 1 calc R U P B 2
C38B C 1.0030(10) 0.1256(7) 0.4445(6) 0.043(2) Uani 0.315(7) 1 d G U P B 2
H38B H 1.092855 0.089626 0.466234 0.051 Uiso 0.315(7) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.3514(7) . ?
Pd1 C6 2.142(2) . ?
Pd1 C8 2.144(2) . ?
Pd1 C9A 2.124(5) . ?
Pd1 C9B 2.136(5) . ?
Pd1 C10 2.109(3) . ?
O1 C7 1.170(3) . ?
N1 C2 1.357(3) . ?
N1 C5 1.389(3) . ?
N1 C11 1.448(3) . ?
N2 C2 1.365(3) . ?
N2 C4 1.382(3) . ?
N2 C23 1.437(3) . ?
C2 C6 1.402(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.344(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.302(3) . ?
C8 H8BC 0.9900 . ?
C8 H8BD 0.9900 . ?
C8 H8AA 0.9900 . ?
C8 H8AB 0.9900 . ?
C8 C9A 1.345(6) . ?
C8 C9B 1.383(7) . ?
C9A H9A 1.0000 . ?
C9A C10 1.401(6) . ?
C9B H9B 1.0000 . ?
C9B C10 1.358(6) . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.404(3) . ?
C11 C16 1.400(3) . ?
C12 C13 1.394(3) . ?
C12 C17 1.517(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.373(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(3) . ?
C16 C20 1.523(3) . ?
C17 H17 1.0000 . ?
C17 C18 1.525(4) . ?
C17 C19 1.534(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 1.0000 . ?
C20 C21 1.525(3) . ?
C20 C22 1.526(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.394(3) . ?
C23 C28 1.402(3) . ?
C24 C25 1.392(4) . ?
C24 C29 1.520(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.380(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.389(4) . ?
C28 C32 1.519(4) . ?
C29 H29 1.0000 . ?
C29 C30 1.523(4) . ?
C29 C31 1.524(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 1.0000 . ?
C32 C33 1.514(4) . ?
C32 C34 1.514(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35A H35A 0.9500 . ?
C35A C36A 1.353(9) . ?
C35A C40A 1.381(8) . ?
C36A H36A 0.9500 . ?
C36A C37A 1.379(9) . ?
C37A H37A 0.9500 . ?
C37A C38A 1.372(9) . ?
C38A H38A 0.9500 . ?
C38A C39A 1.374(8) . ?
C39A H39A 0.9500 . ?
C39A C40A 1.378(7) . ?
C40A H40A 0.9500 . ?
C37B H37B 0.9500 . ?
C37B C36B 1.3900 . ?
C37B C38B 1.3900 . ?
C36B H36B 0.9500 . ?
C36B C35B 1.3900 . ?
C35B H35B 0.9500 . ?
C35B C40B 1.3900 . ?
C40B H40B 0.9500 . ?
C40B C39B 1.3900 . ?
C39B H39B 0.9500 . ?
C39B C38B 1.3900 . ?
C38B H38B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Pd1 Cl1 91.58(6) . . ?
C6 Pd1 C8 171.45(11) . . ?
C8 Pd1 Cl1 96.70(9) . . ?
C9A Pd1 Cl1 129.88(15) . . ?
C9A Pd1 C6 134.77(16) . . ?
C9A Pd1 C8 36.75(17) . . ?
C9B Pd1 Cl1 127.72(16) . . ?
C9B Pd1 C6 135.94(17) . . ?
C9B Pd1 C8 37.72(18) . . ?
C10 Pd1 Cl1 164.94(8) . . ?
C10 Pd1 C6 102.88(10) . . ?
C10 Pd1 C8 69.02(12) . . ?
C10 Pd1 C9A 38.65(18) . . ?
C10 Pd1 C9B 37.31(18) . . ?
C2 N1 C5 110.47(18) . . ?
C2 N1 C11 126.77(19) . . ?
C5 N1 C11 122.46(19) . . ?
C2 N2 C4 109.93(18) . . ?
C2 N2 C23 123.90(19) . . ?
C4 N2 C23 125.15(18) . . ?
N1 C2 N2 105.21(18) . . ?
N1 C2 C6 127.11(19) . . ?
N2 C2 C6 127.7(2) . . ?
N2 C4 H4 126.2 . . ?
C5 C4 N2 107.69(19) . . ?
C5 C4 H4 126.2 . . ?
N1 C5 H5 126.7 . . ?
C4 C5 N1 106.7(2) . . ?
C4 C5 H5 126.7 . . ?
C2 C6 Pd1 123.57(15) . . ?
C7 C6 Pd1 109.47(16) . . ?
C7 C6 C2 123.9(2) . . ?
O1 C7 C6 173.3(2) . . ?
Pd1 C8 H8BC 116.5 . . ?
Pd1 C8 H8BD 116.5 . . ?
Pd1 C8 H8AA 116.5 . . ?
Pd1 C8 H8AB 116.5 . . ?
H8BC C8 H8BD 113.5 . . ?
H8AA C8 H8AB 113.5 . . ?
C9A C8 Pd1 70.8(2) . . ?
C9A C8 H8AA 116.5 . . ?
C9A C8 H8AB 116.5 . . ?
C9B C8 Pd1 70.8(2) . . ?
C9B C8 H8BC 116.5 . . ?
C9B C8 H8BD 116.5 . . ?
Pd1 C9A H9A 117.7 . . ?
C8 C9A Pd1 72.4(2) . . ?
C8 C9A H9A 117.7 . . ?
C8 C9A C10 122.7(4) . . ?
C10 C9A Pd1 70.1(2) . . ?
C10 C9A H9A 117.7 . . ?
Pd1 C9B H9B 117.3 . . ?
C8 C9B Pd1 71.5(3) . . ?
C8 C9B H9B 117.3 . . ?
C10 C9B Pd1 70.3(2) . . ?
C10 C9B C8 123.0(5) . . ?
C10 C9B H9B 117.3 . . ?
Pd1 C10 H10C 116.3 . . ?
Pd1 C10 H10D 116.3 . . ?
Pd1 C10 H10A 116.5 . . ?
Pd1 C10 H10B 116.5 . . ?
C9A C10 Pd1 71.2(2) . . ?
C9A C10 H10A 116.5 . . ?
C9A C10 H10B 116.5 . . ?
C9B C10 Pd1 72.4(3) . . ?
C9B C10 H10C 116.3 . . ?
C9B C10 H10D 116.3 . . ?
H10C C10 H10D 113.3 . . ?
H10A C10 H10B 113.5 . . ?
C12 C11 N1 117.8(2) . . ?
C16 C11 N1 118.44(19) . . ?
C16 C11 C12 123.7(2) . . ?
C11 C12 C17 122.7(2) . . ?
C13 C12 C11 116.3(2) . . ?
C13 C12 C17 121.0(2) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.7(2) . . ?
C14 C13 H13 119.2 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.5(2) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.0(2) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C20 122.4(2) . . ?
C15 C16 C11 116.8(2) . . ?
C15 C16 C20 120.8(2) . . ?
C12 C17 H17 107.8 . . ?
C12 C17 C18 111.6(2) . . ?
C12 C17 C19 111.9(2) . . ?
C18 C17 H17 107.8 . . ?
C18 C17 C19 109.8(2) . . ?
C19 C17 H17 107.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20 107.2 . . ?
C16 C20 C21 111.5(2) . . ?
C16 C20 C22 114.0(2) . . ?
C21 C20 H20 107.2 . . ?
C21 C20 C22 109.4(2) . . ?
C22 C20 H20 107.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N2 119.20(19) . . ?
C24 C23 C28 123.4(2) . . ?
C28 C23 N2 117.4(2) . . ?
C23 C24 C29 122.1(2) . . ?
C25 C24 C23 117.2(2) . . ?
C25 C24 C29 120.7(2) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.8(3) . . ?
C26 C25 H25 119.6 . . ?
C25 C26 H26 119.6 . . ?
C27 C26 C25 120.7(2) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 121.0(2) . . ?
C28 C27 H27 119.5 . . ?
C23 C28 C32 122.0(2) . . ?
C27 C28 C23 116.9(2) . . ?
C27 C28 C32 121.1(2) . . ?
C24 C29 H29 107.9 . . ?
C24 C29 C30 111.7(2) . . ?
C24 C29 C31 110.6(2) . . ?
C30 C29 H29 107.9 . . ?
C30 C29 C31 110.8(2) . . ?
C31 C29 H29 107.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C28 C32 H32 107.1 . . ?
C33 C32 C28 112.7(2) . . ?
C33 C32 H32 107.1 . . ?
C33 C32 C34 111.3(3) . . ?
C34 C32 C28 111.3(3) . . ?
C34 C32 H32 107.1 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36A C35A H35A 120.2 . . ?
C36A C35A C40A 119.7(6) . . ?
C40A C35A H35A 120.2 . . ?
C35A C36A H36A 119.6 . . ?
C35A C36A C37A 120.8(6) . . ?
C37A C36A H36A 119.6 . . ?
C36A C37A H37A 120.1 . . ?
C38A C37A C36A 119.8(5) . . ?
C38A C37A H37A 120.1 . . ?
C37A C38A H38A 120.1 . . ?
C37A C38A C39A 119.9(6) . . ?
C39A C38A H38A 120.1 . . ?
C38A C39A H39A 120.1 . . ?
C38A C39A C40A 119.8(6) . . ?
C40A C39A H39A 120.1 . . ?
C35A C40A H40A 120.0 . . ?
C39A C40A C35A 120.0(5) . . ?
C39A C40A H40A 120.0 . . ?
C36B C37B H37B 120.0 . . ?
C36B C37B C38B 120.0 . . ?
C38B C37B H37B 120.0 . . ?
C37B C36B H36B 120.0 . . ?
C35B C36B C37B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C36B C35B C40B 120.0 . . ?
C40B C35B H35B 120.0 . . ?
C35B C40B H40B 120.0 . . ?
C39B C40B C35B 120.0 . . ?
C39B C40B H40B 120.0 . . ?
C40B C39B H39B 120.0 . . ?
C40B C39B C38B 120.0 . . ?
C38B C39B H39B 120.0 . . ?
C37B C38B H38B 120.0 . . ?
C39B C38B C37B 120.0 . . ?
C39B C38B H38B 120.0 . . ?

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
Pd1 C8 C9A C10 -51.2(4) . . . . ?
Pd1 C8 C9B C10 50.0(4) . . . . ?
N1 C2 C6 Pd1 34.4(3) . . . . ?
N1 C2 C6 C7 -167.3(2) . . . . ?
N1 C11 C12 C13 -175.6(2) . . . . ?
N1 C11 C12 C17 3.5(3) . . . . ?
N1 C11 C16 C15 175.9(2) . . . . ?
N1 C11 C16 C20 -3.3(3) . . . . ?
N2 C2 C6 Pd1 -144.78(17) . . . . ?
N2 C2 C6 C7 13.4(4) . . . . ?
N2 C4 C5 N1 0.3(2) . . . . ?
N2 C23 C24 C25 178.7(2) . . . . ?
N2 C23 C24 C29 -1.8(3) . . . . ?
N2 C23 C28 C27 -179.4(2) . . . . ?
N2 C23 C28 C32 1.9(3) . . . . ?
C2 N1 C5 C4 0.2(2) . . . . ?
C2 N1 C11 C12 -109.3(3) . . . . ?
C2 N1 C11 C16 73.5(3) . . . . ?
C2 N2 C4 C5 -0.7(2) . . . . ?
C2 N2 C23 C24 91.5(3) . . . . ?
C2 N2 C23 C28 -88.1(3) . . . . ?
C4 N2 C2 N1 0.8(2) . . . . ?
C4 N2 C2 C6 -179.9(2) . . . . ?
C4 N2 C23 C24 -101.3(3) . . . . ?
C4 N2 C23 C28 79.1(3) . . . . ?
C5 N1 C2 N2 -0.6(2) . . . . ?
C5 N1 C2 C6 -179.9(2) . . . . ?
C5 N1 C11 C12 77.7(3) . . . . ?
C5 N1 C11 C16 -99.5(3) . . . . ?
C8 C9A C10 Pd1 52.2(4) . . . . ?
C8 C9B C10 Pd1 -50.5(4) . . . . ?
C11 N1 C2 N2 -174.32(19) . . . . ?
C11 N1 C2 C6 6.3(3) . . . . ?
C11 N1 C5 C4 174.23(19) . . . . ?
C11 C12 C13 C14 -0.4(4) . . . . ?
C11 C12 C17 C18 -98.0(3) . . . . ?
C11 C12 C17 C19 138.5(2) . . . . ?
C11 C16 C20 C21 77.8(3) . . . . ?
C11 C16 C20 C22 -157.7(2) . . . . ?
C12 C11 C16 C15 -1.2(3) . . . . ?
C12 C11 C16 C20 179.7(2) . . . . ?
C12 C13 C14 C15 -1.0(4) . . . . ?
C13 C12 C17 C18 81.0(3) . . . . ?
C13 C12 C17 C19 -42.5(3) . . . . ?
C13 C14 C15 C16 1.3(4) . . . . ?
C14 C15 C16 C11 -0.3(4) . . . . ?
C14 C15 C16 C20 178.9(2) . . . . ?
C15 C16 C20 C21 -101.4(3) . . . . ?
C15 C16 C20 C22 23.2(3) . . . . ?
C16 C11 C12 C13 1.5(4) . . . . ?
C16 C11 C12 C17 -179.4(2) . . . . ?
C17 C12 C13 C14 -179.5(2) . . . . ?
C23 N2 C2 N1 169.69(18) . . . . ?
C23 N2 C2 C6 -11.0(3) . . . . ?
C23 N2 C4 C5 -169.4(2) . . . . ?
C23 C24 C25 C26 1.1(4) . . . . ?
C23 C24 C29 C30 -133.8(3) . . . . ?
C23 C24 C29 C31 102.3(3) . . . . ?
C23 C28 C32 C33 -113.2(3) . . . . ?
C23 C28 C32 C34 121.0(3) . . . . ?
C24 C23 C28 C27 1.0(4) . . . . ?
C24 C23 C28 C32 -177.7(2) . . . . ?
C24 C25 C26 C27 0.3(4) . . . . ?
C25 C24 C29 C30 45.7(3) . . . . ?
C25 C24 C29 C31 -78.2(3) . . . . ?
C25 C26 C27 C28 -1.1(4) . . . . ?
C26 C27 C28 C23 0.4(4) . . . . ?
C26 C27 C28 C32 179.2(2) . . . . ?
C27 C28 C32 C33 68.2(3) . . . . ?
C27 C28 C32 C34 -57.6(3) . . . . ?
C28 C23 C24 C25 -1.8(4) . . . . ?
C28 C23 C24 C29 177.8(2) . . . . ?
C29 C24 C25 C26 -178.5(3) . . . . ?
C35A C36A C37A C38A -2.8(9) . . . . ?
C36A C35A C40A C39A 2.1(9) . . . . ?
C36A C37A C38A C39A 2.6(8) . . . . ?
C37A C38A C39A C40A -0.1(8) . . . . ?
C38A C39A C40A C35A -2.3(8) . . . . ?
C40A C35A C36A C37A 0.4(9) . . . . ?
C37B C36B C35B C40B 0.0 . . . . ?
C36B C37B C38B C39B 0.0 . . . . ?
C36B C35B C40B C39B 0.0 . . . . ?
C35B C40B C39B C38B 0.0 . . . . ?
C40B C39B C38B C37B 0.0 . . . . ?
C38B C37B C36B C35B 0.0 . . . . ?

_olex2_date_sample_data_collection 2021-05-12
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.796
####################################################################### 
# 
# 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_wf446mesitol
_database_code_depnum_ccdc_archive 'CCDC 2094465'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-07-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H48 N2 O2'
_chemical_formula_sum            'C38 H48 N2 O2'
_chemical_formula_weight         564.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H48 N2 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   20.58217(16)
_cell_length_b                   16.76993(7)
_cell_length_c                   20.98706(16)
_cell_angle_alpha                90
_cell_angle_beta                 114.7272(9)
_cell_angle_gamma                90
_cell_volume                     6579.72(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    27786
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5590
_cell_measurement_theta_min      3.5150
_shelx_estimated_absorpt_T_max   0.963
_shelx_estimated_absorpt_T_min   0.882
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.1171
0 1 0 0.1267
-1 2 0 0.1394
-2 0 1 0.0969
2 0 -1 0.0928
0 0 -1 0.0382
0 0 1 0.0363
1 0 0 0.0843
-1 0 0 0.0977
2 2 -1 0.1326
0 -1 -2 0.0681

_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0017 -1.0009 0.0001 0.0192 0.0091 0.0894
0.0017 1.0009 -0.0001 -0.0192 -0.0091 -0.0894
-0.9980 2.0030 0.0025 0.0340 0.0163 -0.1979
-2.0012 0.0018 1.0041 0.1468 -0.0116 -0.0303
2.0012 -0.0018 -1.0041 -0.1468 0.0116 0.0303
-0.0014 0.0005 -0.9989 -0.0018 0.0804 -0.0078
0.0014 -0.0005 0.9989 0.0018 -0.0804 0.0078
1.0013 -0.0012 -0.0026 -0.0725 -0.0344 0.0190
-1.0013 0.0012 0.0026 0.0725 0.0344 -0.0190
2.0046 2.0001 -1.0042 -0.1852 -0.0066 -0.1485
-0.0046 -0.9999 -1.9977 0.0156 0.1699 0.0739

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.739
_diffrn_reflns_theta_min         3.510
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -112.00 -87.00   1.00    3.00    --  -41.04-149.00-112.00   25
  2  ω    -85.00 -60.00   1.00    3.00    --  -41.04 149.00 -65.00   25
  3  ω    -74.00  -4.00   1.00    3.00    --  -41.04 123.00 131.00   70
  4  ω     52.00  77.00   1.00    3.00    --   41.04-149.00-112.00   25
  5  ω     60.00  85.00   1.00    3.00    --   41.04-123.00  51.00   25
  6  ω     74.00 128.00   1.00   12.00    --  105.15-149.00-112.00   54
  7  ω     47.00  74.00   1.00   12.00    --  105.15-123.00  51.00   27
  8  ω    112.00 145.00   1.00   12.00    --  105.15 123.00 131.00   33
  9  ω    100.00 126.00   1.00   12.00    --  105.15 149.00 -65.00   26
 10  ω    -35.00  -8.00   1.00    3.00    --  -41.04 125.00-180.00   27
 11  ω   -111.00 -18.00   1.00    3.00    --  -41.04 -38.00  30.00   93
 12  ω   -102.00 -18.00   1.00    3.00    --  -41.04 -38.00 -60.00   84
 13  ω     37.00  62.00   1.00    3.00    --   41.04  38.00  60.00   25
 14  ω     23.00  97.00   1.00    3.00    --   41.04  57.00 120.00   74
 15  ω     14.00  81.00   1.00    3.00    --   41.04 -99.00 -90.00   67
 16  ω    110.00 165.00   1.00   12.00    --  105.15  77.00-180.00   55
 17  ω     32.00 109.00   1.00   12.00    --  105.15-111.00 -30.00   77
 18  ω     80.00 176.00   1.00   12.00    --  105.15  45.00 120.00   96
 19  ω     34.00  91.00   1.00   12.00    --  105.15 -94.00   0.00   57
 20  ω     31.00 107.00   1.00   12.00    --  105.15-111.00-120.00   76
 21  ω     73.00 109.00   1.00   12.00    --  105.15-111.00  90.00   36
 22  ω     30.00  79.00   1.00   12.00    --  105.15-111.00 -60.00   49
 23  ω     34.00 134.00   1.00   12.00    --  105.15 -61.00  30.00  100
 24  ω     84.00 109.00   1.00   12.00    --  105.15-111.00 120.00   25
 25  ω     88.00 146.00   1.00   12.00    --  105.15  45.00-180.00   58
 26  ω    105.00 164.00   1.00   12.00    --  105.15 111.00   0.00   59
 27  ω     95.00 171.00   1.00   12.00    --  105.15  61.00  60.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0723879000
_diffrn_orient_matrix_UB_12      -0.0190940000
_diffrn_orient_matrix_UB_13      0.0019153000
_diffrn_orient_matrix_UB_21      -0.0345928000
_diffrn_orient_matrix_UB_22      -0.0089963000
_diffrn_orient_matrix_UB_23      -0.0804447000
_diffrn_orient_matrix_UB_31      0.0189267000
_diffrn_orient_matrix_UB_32      -0.0893730000
_diffrn_orient_matrix_UB_33      0.0076935000
_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                11527
_reflns_number_total             12907
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.00022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         12907
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²+2.1889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1017
_refine_special_details          ?
_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:
 C23(H23), C26(H26), C35(H35), C38(H38), C63(H63), C66(H66), C75(H75), C78(H78)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C19(H19), C20(H20), C21(H21),
 C31(H31), C32(H32), C33(H33), C44(H44), C45(H45), C46(H46), C50(H50), C52(H52),
  C59(H59), C60(H60), C61(H61), C71(H71), C72(H72), C73(H73)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C76(H76A,
 H76B,H76C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.23552(5) 0.71811(5) 0.69960(4) 0.0328(2) Uani 1 1 d . . . . .
O2 O 0.15193(5) 0.71628(5) 0.58649(4) 0.02866(19) Uani 1 1 d . . . . .
N1 N 0.25925(5) 0.52908(5) 0.75567(5) 0.02029(19) Uani 1 1 d . . . . .
N2 N 0.20471(5) 0.45426(5) 0.66349(5) 0.02020(19) Uani 1 1 d . . . . .
C2 C 0.21565(6) 0.53248(6) 0.68562(6) 0.0196(2) Uani 1 1 d . . . . .
C4 C 0.24104(6) 0.40344(6) 0.72018(6) 0.0214(2) Uani 1 1 d . . . . .
H4 H 0.241585 0.346824 0.718839 0.026 Uiso 1 1 calc R U . . .
C5 C 0.27472(6) 0.44911(6) 0.77640(6) 0.0218(2) Uani 1 1 d . . . . .
H5 H 0.304037 0.430825 0.822386 0.026 Uiso 1 1 calc R U . . .
C6 C 0.18388(6) 0.59548(7) 0.64019(6) 0.0226(2) Uani 1 1 d . . . . .
H6 H 0.148371 0.580419 0.595560 0.027 Uiso 1 1 calc R U . . .
C7 C 0.19611(6) 0.67858(7) 0.64997(6) 0.0243(2) Uani 1 1 d . . . . .
C8 C 0.16438(7) 0.79558(7) 0.57525(6) 0.0253(2) Uani 1 1 d . . . . .
C9 C 0.22677(7) 0.81780(7) 0.56909(6) 0.0280(3) Uani 1 1 d . . . . .
C10 C 0.22939(7) 0.89479(7) 0.54465(6) 0.0298(3) Uani 1 1 d . . . . .
H10 H 0.271532 0.911313 0.540360 0.036 Uiso 1 1 calc R U . . .
C11 C 0.17272(7) 0.94805(7) 0.52640(6) 0.0296(3) Uani 1 1 d . . . . .
C12 C 0.11290(7) 0.92401(7) 0.53596(6) 0.0287(3) Uani 1 1 d . . . . .
H12 H 0.074412 0.960393 0.525489 0.034 Uiso 1 1 calc R U . . .
C13 C 0.10752(7) 0.84812(7) 0.56047(6) 0.0268(2) Uani 1 1 d . . . . .
C14 C 0.28777(8) 0.76063(8) 0.58436(7) 0.0362(3) Uani 1 1 d . . . . .
H14A H 0.319405 0.780973 0.563839 0.054 Uiso 1 1 calc R U . . .
H14B H 0.268918 0.708456 0.563969 0.054 Uiso 1 1 calc R U . . .
H14C H 0.314747 0.755208 0.635233 0.054 Uiso 1 1 calc R U . . .
C15 C 0.17494(9) 1.02849(8) 0.49521(7) 0.0399(3) Uani 1 1 d . . . . .
H15A H 0.132044 1.035329 0.451339 0.060 Uiso 1 1 calc R U . . .
H15B H 0.217587 1.031915 0.485683 0.060 Uiso 1 1 calc R U . . .
H15C H 0.176651 1.070490 0.528343 0.060 Uiso 1 1 calc R U . . .
C16 C 0.04143(8) 0.82224(8) 0.56846(8) 0.0376(3) Uani 1 1 d . . . . .
H16A H 0.015813 0.782306 0.532624 0.056 Uiso 1 1 calc R U . . .
H16B H 0.010366 0.868471 0.562804 0.056 Uiso 1 1 calc R U . . .
H16C H 0.055009 0.799078 0.615156 0.056 Uiso 1 1 calc R U . . .
C17 C 0.28586(6) 0.59379(6) 0.80511(6) 0.0228(2) Uani 1 1 d . . . . .
C18 C 0.35894(7) 0.61097(7) 0.83168(6) 0.0271(2) Uani 1 1 d . . . . .
C19 C 0.38472(8) 0.67111(8) 0.88216(7) 0.0347(3) Uani 1 1 d . . . . .
H19 H 0.434191 0.684056 0.901853 0.042 Uiso 1 1 calc R U . . .
C20 C 0.33940(9) 0.71195(8) 0.90381(7) 0.0378(3) Uani 1 1 d . . . . .
H20 H 0.357891 0.752603 0.938277 0.045 Uiso 1 1 calc R U . . .
C21 C 0.26710(8) 0.69411(7) 0.87567(7) 0.0347(3) Uani 1 1 d . . . . .
H21 H 0.236522 0.723364 0.890704 0.042 Uiso 1 1 calc R U . . .
C22 C 0.23824(7) 0.63401(7) 0.82567(6) 0.0271(2) Uani 1 1 d . . . . .
C23 C 0.40739(7) 0.56989(7) 0.80370(7) 0.0312(3) Uani 1 1 d . . . . .
H23 H 0.383507 0.518921 0.781305 0.037 Uiso 1 1 calc R U . . .
C24 C 0.41500(10) 0.62025(10) 0.74672(8) 0.0483(4) Uani 1 1 d . . . . .
H24A H 0.436822 0.671615 0.766526 0.072 Uiso 1 1 calc R U . . .
H24B H 0.367669 0.629279 0.708567 0.072 Uiso 1 1 calc R U . . .
H24C H 0.445390 0.592220 0.728429 0.072 Uiso 1 1 calc R U . . .
C25 C 0.48068(8) 0.54843(11) 0.86022(9) 0.0487(4) Uani 1 1 d . . . . .
H25A H 0.507660 0.518555 0.839148 0.073 Uiso 1 1 calc R U . . .
H25B H 0.474930 0.515589 0.896140 0.073 Uiso 1 1 calc R U . . .
H25C H 0.506650 0.597329 0.881764 0.073 Uiso 1 1 calc R U . . .
C26 C 0.15957(7) 0.61163(8) 0.79610(7) 0.0305(3) Uani 1 1 d . . . . .
H26 H 0.145731 0.591660 0.747256 0.037 Uiso 1 1 calc R U . . .
C27 C 0.11070(9) 0.68190(10) 0.79177(10) 0.0498(4) Uani 1 1 d . . . . .
H27A H 0.118914 0.698801 0.839232 0.075 Uiso 1 1 calc R U . . .
H27B H 0.060667 0.665694 0.766117 0.075 Uiso 1 1 calc R U . . .
H27C H 0.121166 0.726300 0.767164 0.075 Uiso 1 1 calc R U . . .
C28 C 0.14787(8) 0.54333(9) 0.83853(7) 0.0372(3) Uani 1 1 d . . . . .
H28A H 0.176285 0.497046 0.837066 0.056 Uiso 1 1 calc R U . . .
H28B H 0.097090 0.528872 0.818406 0.056 Uiso 1 1 calc R U . . .
H28C H 0.162762 0.560336 0.887302 0.056 Uiso 1 1 calc R U . . .
C29 C 0.14619(6) 0.42938(6) 0.59953(6) 0.0219(2) Uani 1 1 d . . . . .
C30 C 0.08086(6) 0.41237(7) 0.60314(6) 0.0265(2) Uani 1 1 d . . . . .
C31 C 0.02408(7) 0.38767(8) 0.54175(7) 0.0338(3) Uani 1 1 d . . . . .
H31 H -0.020611 0.375081 0.542459 0.041 Uiso 1 1 calc R U . . .
C32 C 0.03210(8) 0.38129(8) 0.47978(7) 0.0358(3) Uani 1 1 d . . . . .
H32 H -0.007108 0.364261 0.438321 0.043 Uiso 1 1 calc R U . . .
C33 C 0.09664(7) 0.39944(7) 0.47753(6) 0.0314(3) Uani 1 1 d . . . . .
H33 H 0.101005 0.394790 0.434379 0.038 Uiso 1 1 calc R U . . .
C34 C 0.15567(7) 0.42454(6) 0.53754(6) 0.0252(2) Uani 1 1 d . . . . .
C35 C 0.07282(7) 0.42088(8) 0.67169(7) 0.0298(3) Uani 1 1 d . . . . .
H35 H 0.111622 0.457406 0.702575 0.036 Uiso 1 1 calc R U . . .
C36 C 0.00164(8) 0.45797(10) 0.66232(9) 0.0451(4) Uani 1 1 d . . . . .
H36A H -0.002624 0.511289 0.641834 0.068 Uiso 1 1 calc R U . . .
H36B H -0.000355 0.462039 0.708048 0.068 Uiso 1 1 calc R U . . .
H36C H -0.037776 0.424397 0.631063 0.068 Uiso 1 1 calc R U . . .
C37 C 0.08310(8) 0.34103(8) 0.71015(7) 0.0367(3) Uani 1 1 d . . . . .
H37A H 0.043790 0.304972 0.682884 0.055 Uiso 1 1 calc R U . . .
H37B H 0.083443 0.349801 0.756455 0.055 Uiso 1 1 calc R U . . .
H37C H 0.128655 0.317220 0.715717 0.055 Uiso 1 1 calc R U . . .
C38 C 0.22527(7) 0.44696(8) 0.53348(6) 0.0294(3) Uani 1 1 d . . . . .
H38 H 0.261646 0.457994 0.582204 0.035 Uiso 1 1 calc R U . . .
C39 C 0.21660(9) 0.52269(8) 0.48974(8) 0.0399(3) Uani 1 1 d . . . . .
H39A H 0.181660 0.513032 0.441464 0.060 Uiso 1 1 calc R U . . .
H39B H 0.262770 0.537056 0.489767 0.060 Uiso 1 1 calc R U . . .
H39C H 0.199845 0.566400 0.510028 0.060 Uiso 1 1 calc R U . . .
C40 C 0.25344(9) 0.37909(9) 0.50341(8) 0.0419(3) Uani 1 1 d . . . . .
H40A H 0.256905 0.330256 0.530296 0.063 Uiso 1 1 calc R U . . .
H40B H 0.300857 0.393162 0.506434 0.063 Uiso 1 1 calc R U . . .
H40C H 0.220619 0.370318 0.454214 0.063 Uiso 1 1 calc R U . . .
O3 O 0.23295(5) 0.10985(5) 0.29249(7) 0.0478(3) Uani 1 1 d . . . . .
O4 O 0.18311(4) 0.23147(5) 0.25765(5) 0.0326(2) Uani 1 1 d . . . . .
N3 N 0.42545(5) 0.23940(5) 0.30671(5) 0.02076(19) Uani 1 1 d . . . . .
N4 N 0.40674(5) 0.12374(6) 0.34320(5) 0.0228(2) Uani 1 1 d . . . . .
C42 C 0.37360(6) 0.19418(6) 0.31474(6) 0.0205(2) Uani 1 1 d . . . . .
C44 C 0.47816(6) 0.12667(7) 0.35294(6) 0.0267(2) Uani 1 1 d . . . . .
H44 H 0.512550 0.085440 0.372051 0.032 Uiso 1 1 calc R U . . .
C45 C 0.48952(6) 0.19785(7) 0.33057(6) 0.0243(2) Uani 1 1 d . . . . .
H45 H 0.533295 0.216426 0.330960 0.029 Uiso 1 1 calc R U . . .
C46 C 0.30470(6) 0.22292(7) 0.29592(6) 0.0242(2) Uani 1 1 d . . . . .
H46 H 0.298996 0.279023 0.289921 0.029 Uiso 1 1 calc R U . . .
C47 C 0.24224(6) 0.17952(7) 0.28459(7) 0.0264(2) Uani 1 1 d . . . . .
C48 C 0.11586(6) 0.19787(7) 0.24046(7) 0.0281(3) Uani 1 1 d . . . . .
C49 C 0.07310(7) 0.18260(7) 0.17020(7) 0.0303(3) Uani 1 1 d . . . . .
C50 C 0.00419(7) 0.15354(7) 0.15274(7) 0.0331(3) Uani 1 1 d . . . . .
H50 H -0.026156 0.143456 0.104883 0.040 Uiso 1 1 calc R U . . .
C51 C -0.02120(7) 0.13897(7) 0.20332(8) 0.0336(3) Uani 1 1 d . . . . .
C52 C 0.02315(7) 0.15553(8) 0.27250(8) 0.0345(3) Uani 1 1 d . . . . .
H52 H 0.006168 0.145968 0.307506 0.041 Uiso 1 1 calc R U . . .
C53 C 0.09213(7) 0.18586(7) 0.29266(7) 0.0317(3) Uani 1 1 d . . . . .
C54 C 0.10046(9) 0.19565(10) 0.11498(8) 0.0446(3) Uani 1 1 d . . . . .
H54A H 0.118195 0.250403 0.118160 0.067 Uiso 1 1 calc R U . . .
H54B H 0.061597 0.186921 0.068491 0.067 Uiso 1 1 calc R U . . .
H54C H 0.139449 0.158143 0.122255 0.067 Uiso 1 1 calc R U . . .
C55 C -0.09514(8) 0.10527(9) 0.18295(10) 0.0478(4) Uani 1 1 d . . . . .
H55A H -0.129653 0.135619 0.143345 0.072 Uiso 1 1 calc R U . . .
H55B H -0.107916 0.109054 0.222895 0.072 Uiso 1 1 calc R U . . .
H55C H -0.095911 0.049251 0.169368 0.072 Uiso 1 1 calc R U . . .
C56 C 0.13935(9) 0.20477(10) 0.36797(8) 0.0471(4) Uani 1 1 d . . . . .
H56A H 0.177650 0.165033 0.386536 0.071 Uiso 1 1 calc R U . . .
H56B H 0.110893 0.203740 0.395506 0.071 Uiso 1 1 calc R U . . .
H56C H 0.160303 0.257884 0.370991 0.071 Uiso 1 1 calc R U . . .
C57 C 0.41090(6) 0.31605(6) 0.27262(6) 0.0210(2) Uani 1 1 d . . . . .
C58 C 0.37872(6) 0.31822(7) 0.19916(6) 0.0223(2) Uani 1 1 d . . . . .
C59 C 0.35918(7) 0.39280(7) 0.16761(6) 0.0262(2) Uani 1 1 d . . . . .
H59 H 0.337093 0.396478 0.117885 0.031 Uiso 1 1 calc R U . . .
C60 C 0.37133(7) 0.46162(7) 0.20735(7) 0.0296(3) Uani 1 1 d . . . . .
H60 H 0.356410 0.511746 0.184853 0.035 Uiso 1 1 calc R U . . .
C61 C 0.40509(7) 0.45758(7) 0.27960(7) 0.0306(3) Uani 1 1 d . . . . .
H61 H 0.414507 0.505383 0.306267 0.037 Uiso 1 1 calc R U . . .
C62 C 0.42563(7) 0.38459(7) 0.31422(6) 0.0260(2) Uani 1 1 d . . . . .
C63 C 0.36377(7) 0.24337(7) 0.15433(6) 0.0274(2) Uani 1 1 d . . . . .
H63 H 0.387726 0.197427 0.185772 0.033 Uiso 1 1 calc R U . . .
C64 C 0.39417(7) 0.25030(8) 0.09951(7) 0.0326(3) Uani 1 1 d . . . . .
H64A H 0.371271 0.295010 0.068019 0.049 Uiso 1 1 calc R U . . .
H64B H 0.384878 0.200809 0.072286 0.049 Uiso 1 1 calc R U . . .
H64C H 0.445864 0.259531 0.123026 0.049 Uiso 1 1 calc R U . . .
C65 C 0.28352(8) 0.22590(10) 0.11823(8) 0.0438(4) Uani 1 1 d . . . . .
H65A H 0.264135 0.222485 0.153577 0.066 Uiso 1 1 calc R U . . .
H65B H 0.275695 0.175176 0.092901 0.066 Uiso 1 1 calc R U . . .
H65C H 0.259338 0.268837 0.085092 0.066 Uiso 1 1 calc R U . . .
C66 C 0.46202(8) 0.38095(8) 0.39377(7) 0.0334(3) Uani 1 1 d . . . . .
H66 H 0.468523 0.323452 0.407673 0.040 Uiso 1 1 calc R U . . .
C67 C 0.53591(11) 0.41906(13) 0.42112(9) 0.0648(5) Uani 1 1 d . . . . .
H67A H 0.565136 0.391194 0.401369 0.097 Uiso 1 1 calc R U . . .
H67B H 0.558896 0.415208 0.472399 0.097 Uiso 1 1 calc R U . . .
H67C H 0.531239 0.475280 0.407169 0.097 Uiso 1 1 calc R U . . .
C68 C 0.41640(12) 0.41880(16) 0.42657(9) 0.0741(6) Uani 1 1 d . . . . .
H68A H 0.409309 0.475408 0.413952 0.111 Uiso 1 1 calc R U . . .
H68B H 0.440514 0.413524 0.477711 0.111 Uiso 1 1 calc R U . . .
H68C H 0.369894 0.391921 0.409253 0.111 Uiso 1 1 calc R U . . .
C69 C 0.37968(6) 0.05851(6) 0.37000(6) 0.0222(2) Uani 1 1 d . . . . .
C70 C 0.35260(6) -0.00853(7) 0.32755(6) 0.0246(2) Uani 1 1 d . . . . .
C71 C 0.32979(7) -0.07206(7) 0.35577(7) 0.0282(3) Uani 1 1 d . . . . .
H71 H 0.311168 -0.118639 0.328425 0.034 Uiso 1 1 calc R U . . .
C72 C 0.33397(7) -0.06806(7) 0.42317(7) 0.0313(3) Uani 1 1 d . . . . .
H72 H 0.317993 -0.111799 0.441613 0.038 Uiso 1 1 calc R U . . .
C73 C 0.36116(7) -0.00107(7) 0.46391(7) 0.0300(3) Uani 1 1 d . . . . .
H73 H 0.363529 0.000649 0.510081 0.036 Uiso 1 1 calc R U . . .
C74 C 0.38523(6) 0.06420(7) 0.43848(6) 0.0252(2) Uani 1 1 d . . . . .
C75 C 0.34724(7) -0.01333(7) 0.25315(6) 0.0303(3) Uani 1 1 d . . . . .
H75 H 0.359573 0.040221 0.240358 0.036 Uiso 1 1 calc R U . . .
C76 C 0.27126(9) -0.03418(12) 0.20079(8) 0.0518(4) Uani 1 1 d . . . . .
H76A H 0.259553 -0.088427 0.209867 0.078 Uiso 1 1 calc R U . . .
H76B H 0.268118 -0.031008 0.152955 0.078 Uiso 1 1 calc R U . . .
H76C H 0.237421 0.003528 0.205977 0.078 Uiso 1 1 calc R U . . .
C77 C 0.40042(9) -0.07382(9) 0.24851(8) 0.0413(3) Uani 1 1 d . . . . .
H77A H 0.448972 -0.058947 0.281411 0.062 Uiso 1 1 calc R U . . .
H77B H 0.397417 -0.074447 0.200662 0.062 Uiso 1 1 calc R U . . .
H77C H 0.389037 -0.126929 0.260472 0.062 Uiso 1 1 calc R U . . .
C78 C 0.41492(7) 0.13753(7) 0.48401(7) 0.0299(3) Uani 1 1 d . . . . .
H78 H 0.438575 0.171531 0.460715 0.036 Uiso 1 1 calc R U . . .
C79 C 0.47127(8) 0.11595(9) 0.55691(7) 0.0391(3) Uani 1 1 d . . . . .
H79A H 0.448893 0.085170 0.582056 0.059 Uiso 1 1 calc R U . . .
H79B H 0.492081 0.164860 0.583046 0.059 Uiso 1 1 calc R U . . .
H79C H 0.508991 0.083984 0.552417 0.059 Uiso 1 1 calc R U . . .
C80 C 0.35450(8) 0.18667(8) 0.48925(8) 0.0396(3) Uani 1 1 d . . . . .
H80A H 0.320757 0.203152 0.442187 0.059 Uiso 1 1 calc R U . . .
H80B H 0.374676 0.234024 0.518149 0.059 Uiso 1 1 calc R U . . .
H80C H 0.329451 0.154214 0.510757 0.059 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
O1 C7 1.2147(15) . ?
O2 C7 1.4099(14) . ?
O2 C8 1.3930(14) . ?
N1 C2 1.3660(14) . ?
N1 C5 1.4047(14) . ?
N1 C17 1.4418(14) . ?
N2 C2 1.3783(14) . ?
N2 C4 1.3987(14) . ?
N2 C29 1.4401(14) . ?
C2 C6 1.3897(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.3324(16) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C6 C7 1.4158(16) . ?
C8 C9 1.3941(18) . ?
C8 C13 1.3921(18) . ?
C9 C10 1.3986(17) . ?
C9 C14 1.5040(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.3898(19) . ?
C11 C12 1.3875(19) . ?
C11 C15 1.5085(17) . ?
C12 H12 0.9500 . ?
C12 C13 1.3943(17) . ?
C13 C16 1.5026(18) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.3980(17) . ?
C17 C22 1.3984(17) . ?
C18 C19 1.3968(17) . ?
C18 C23 1.5178(18) . ?
C19 H19 0.9500 . ?
C19 C20 1.379(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.385(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.3959(17) . ?
C22 C26 1.5190(19) . ?
C23 H23 1.0000 . ?
C23 C24 1.525(2) . ?
C23 C25 1.5214(19) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.5271(18) . ?
C26 C28 1.5304(18) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.4073(17) . ?
C29 C34 1.3962(16) . ?
C30 C31 1.3919(17) . ?
C30 C35 1.5221(17) . ?
C31 H31 0.9500 . ?
C31 C32 1.382(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.383(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.3998(17) . ?
C34 C38 1.5177(18) . ?
C35 H35 1.0000 . ?
C35 C36 1.5267(19) . ?
C35 C37 1.5319(17) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 1.0000 . ?
C38 C39 1.5331(18) . ?
C38 C40 1.5285(18) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O3 C47 1.2066(15) . ?
O4 C47 1.4087(14) . ?
O4 C48 1.3948(14) . ?
N3 C42 1.3757(14) . ?
N3 C45 1.3867(15) . ?
N3 C57 1.4403(14) . ?
N4 C42 1.3699(14) . ?
N4 C44 1.3976(15) . ?
N4 C69 1.4441(14) . ?
C42 C46 1.3896(16) . ?
C44 H44 0.9500 . ?
C44 C45 1.3386(17) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C46 C47 1.4082(16) . ?
C48 C49 1.3886(19) . ?
C48 C53 1.3882(19) . ?
C49 C50 1.3960(18) . ?
C49 C54 1.5013(19) . ?
C50 H50 0.9500 . ?
C50 C51 1.387(2) . ?
C51 C52 1.382(2) . ?
C51 C55 1.5079(18) . ?
C52 H52 0.9500 . ?
C52 C53 1.3967(18) . ?
C53 C56 1.503(2) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.4010(16) . ?
C57 C62 1.3979(16) . ?
C58 C59 1.3934(16) . ?
C58 C63 1.5209(16) . ?
C59 H59 0.9500 . ?
C59 C60 1.3841(17) . ?
C60 H60 0.9500 . ?
C60 C61 1.3803(19) . ?
C61 H61 0.9500 . ?
C61 C62 1.3957(17) . ?
C62 C66 1.5185(17) . ?
C63 H63 1.0000 . ?
C63 C64 1.5269(17) . ?
C63 C65 1.5300(19) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66 1.0000 . ?
C66 C67 1.523(2) . ?
C66 C68 1.516(2) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 C70 1.3975(16) . ?
C69 C74 1.3965(16) . ?
C70 C71 1.3925(16) . ?
C70 C75 1.5206(16) . ?
C71 H71 0.9500 . ?
C71 C72 1.3823(18) . ?
C72 H72 0.9500 . ?
C72 C73 1.3806(18) . ?
C73 H73 0.9500 . ?
C73 C74 1.3964(17) . ?
C74 C78 1.5199(17) . ?
C75 H75 1.0000 . ?
C75 C76 1.529(2) . ?
C75 C77 1.5250(19) . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78 1.0000 . ?
C78 C79 1.5273(19) . ?
C78 C80 1.5337(18) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 O2 C7 119.77(9) . . ?
C2 N1 C5 109.57(9) . . ?
C2 N1 C17 128.60(9) . . ?
C5 N1 C17 121.80(9) . . ?
C2 N2 C4 109.85(9) . . ?
C2 N2 C29 123.01(9) . . ?
C4 N2 C29 123.87(9) . . ?
N1 C2 N2 105.31(9) . . ?
N1 C2 C6 132.76(10) . . ?
N2 C2 C6 121.92(10) . . ?
N2 C4 H4 126.3 . . ?
C5 C4 N2 107.33(9) . . ?
C5 C4 H4 126.3 . . ?
N1 C5 H5 126.0 . . ?
C4 C5 N1 107.94(10) . . ?
C4 C5 H5 126.0 . . ?
C2 C6 H6 114.9 . . ?
C2 C6 C7 130.15(11) . . ?
C7 C6 H6 114.9 . . ?
O1 C7 O2 120.06(10) . . ?
O1 C7 C6 132.53(11) . . ?
O2 C7 C6 107.40(10) . . ?
O2 C8 C9 120.85(11) . . ?
C13 C8 O2 116.42(11) . . ?
C13 C8 C9 122.08(11) . . ?
C8 C9 C10 117.33(12) . . ?
C8 C9 C14 121.95(11) . . ?
C10 C9 C14 120.65(12) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 C9 122.52(12) . . ?
C11 C10 H10 118.7 . . ?
C10 C11 C15 121.33(13) . . ?
C12 C11 C10 117.82(11) . . ?
C12 C11 C15 120.83(12) . . ?
C11 C12 H12 119.0 . . ?
C11 C12 C13 122.05(12) . . ?
C13 C12 H12 119.0 . . ?
C8 C13 C12 118.09(12) . . ?
C8 C13 C16 120.54(11) . . ?
C12 C13 C16 121.33(12) . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N1 117.62(10) . . ?
C18 C17 C22 123.60(11) . . ?
C22 C17 N1 118.74(11) . . ?
C17 C18 C23 121.57(10) . . ?
C19 C18 C17 117.09(12) . . ?
C19 C18 C23 121.23(12) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 120.93(13) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.45(12) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.3 . . ?
C20 C21 C22 121.34(12) . . ?
C22 C21 H21 119.3 . . ?
C17 C22 C26 121.32(11) . . ?
C21 C22 C17 116.58(12) . . ?
C21 C22 C26 122.08(12) . . ?
C18 C23 H23 107.2 . . ?
C18 C23 C24 110.59(11) . . ?
C18 C23 C25 113.79(12) . . ?
C24 C23 H23 107.2 . . ?
C25 C23 H23 107.2 . . ?
C25 C23 C24 110.42(12) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26 107.4 . . ?
C22 C26 C27 113.37(12) . . ?
C22 C26 C28 110.34(10) . . ?
C27 C26 H26 107.4 . . ?
C27 C26 C28 110.63(12) . . ?
C28 C26 H26 107.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N2 117.00(10) . . ?
C34 C29 N2 119.81(10) . . ?
C34 C29 C30 123.18(11) . . ?
C29 C30 C35 121.06(11) . . ?
C31 C30 C29 117.50(12) . . ?
C31 C30 C35 121.44(11) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 C30 120.64(12) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 119.7 . . ?
C31 C32 C33 120.65(12) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 119.3 . . ?
C32 C33 C34 121.34(12) . . ?
C34 C33 H33 119.3 . . ?
C29 C34 C33 116.68(11) . . ?
C29 C34 C38 122.75(10) . . ?
C33 C34 C38 120.55(11) . . ?
C30 C35 H35 107.3 . . ?
C30 C35 C36 113.22(11) . . ?
C30 C35 C37 111.74(11) . . ?
C36 C35 H35 107.3 . . ?
C36 C35 C37 109.73(11) . . ?
C37 C35 H35 107.3 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38 108.0 . . ?
C34 C38 C39 111.28(11) . . ?
C34 C38 C40 111.63(11) . . ?
C39 C38 H38 108.0 . . ?
C40 C38 H38 108.0 . . ?
C40 C38 C39 109.81(11) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C48 O4 C47 116.82(9) . . ?
C42 N3 C45 110.37(9) . . ?
C42 N3 C57 122.82(9) . . ?
C45 N3 C57 126.62(9) . . ?
C42 N4 C44 109.56(9) . . ?
C42 N4 C69 128.33(9) . . ?
C44 N4 C69 121.54(9) . . ?
N3 C42 C46 121.72(10) . . ?
N4 C42 N3 104.98(9) . . ?
N4 C42 C46 133.30(10) . . ?
N4 C44 H44 126.0 . . ?
C45 C44 N4 107.90(10) . . ?
C45 C44 H44 126.0 . . ?
N3 C45 H45 126.4 . . ?
C44 C45 N3 107.18(10) . . ?
C44 C45 H45 126.4 . . ?
C42 C46 H46 115.8 . . ?
C42 C46 C47 128.31(10) . . ?
C47 C46 H46 115.8 . . ?
O3 C47 O4 119.60(11) . . ?
O3 C47 C46 131.55(11) . . ?
C46 C47 O4 108.83(9) . . ?
C49 C48 O4 117.96(11) . . ?
C53 C48 O4 119.54(12) . . ?
C53 C48 C49 122.36(11) . . ?
C48 C49 C50 117.79(12) . . ?
C48 C49 C54 121.13(12) . . ?
C50 C49 C54 121.07(13) . . ?
C49 C50 H50 119.1 . . ?
C51 C50 C49 121.82(13) . . ?
C51 C50 H50 119.1 . . ?
C50 C51 C55 120.51(14) . . ?
C52 C51 C50 118.29(12) . . ?
C52 C51 C55 121.20(14) . . ?
C51 C52 H52 118.9 . . ?
C51 C52 C53 122.18(13) . . ?
C53 C52 H52 118.9 . . ?
C48 C53 C52 117.54(12) . . ?
C48 C53 C56 120.88(12) . . ?
C52 C53 C56 121.58(13) . . ?
C49 C54 H54A 109.5 . . ?
C49 C54 H54B 109.5 . . ?
C49 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C51 C55 H55A 109.5 . . ?
C51 C55 H55B 109.5 . . ?
C51 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C57 N3 118.31(10) . . ?
C62 C57 N3 118.55(10) . . ?
C62 C57 C58 123.03(10) . . ?
C57 C58 C63 122.64(10) . . ?
C59 C58 C57 117.13(10) . . ?
C59 C58 C63 120.22(10) . . ?
C58 C59 H59 119.4 . . ?
C60 C59 C58 121.24(11) . . ?
C60 C59 H59 119.4 . . ?
C59 C60 H60 119.9 . . ?
C61 C60 C59 120.14(11) . . ?
C61 C60 H60 119.9 . . ?
C60 C61 H61 119.4 . . ?
C60 C61 C62 121.24(11) . . ?
C62 C61 H61 119.4 . . ?
C57 C62 C66 122.14(11) . . ?
C61 C62 C57 117.18(11) . . ?
C61 C62 C66 120.69(11) . . ?
C58 C63 H63 108.1 . . ?
C58 C63 C64 111.26(10) . . ?
C58 C63 C65 111.20(10) . . ?
C64 C63 H63 108.1 . . ?
C64 C63 C65 109.83(11) . . ?
C65 C63 H63 108.1 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C62 C66 H66 107.7 . . ?
C62 C66 C67 110.66(12) . . ?
C67 C66 H66 107.7 . . ?
C68 C66 C62 111.59(12) . . ?
C68 C66 H66 107.7 . . ?
C68 C66 C67 111.32(15) . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C70 C69 N4 118.48(10) . . ?
C74 C69 N4 118.05(10) . . ?
C74 C69 C70 123.39(10) . . ?
C69 C70 C75 122.38(10) . . ?
C71 C70 C69 117.37(11) . . ?
C71 C70 C75 120.25(11) . . ?
C70 C71 H71 119.7 . . ?
C72 C71 C70 120.69(11) . . ?
C72 C71 H71 119.7 . . ?
C71 C72 H72 119.7 . . ?
C73 C72 C71 120.59(11) . . ?
C73 C72 H72 119.7 . . ?
C72 C73 H73 119.4 . . ?
C72 C73 C74 121.19(11) . . ?
C74 C73 H73 119.4 . . ?
C69 C74 C78 122.72(10) . . ?
C73 C74 C69 116.77(11) . . ?
C73 C74 C78 120.51(11) . . ?
C70 C75 H75 108.1 . . ?
C70 C75 C76 111.30(11) . . ?
C70 C75 C77 110.80(11) . . ?
C76 C75 H75 108.1 . . ?
C77 C75 H75 108.1 . . ?
C77 C75 C76 110.34(12) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C74 C78 H78 107.7 . . ?
C74 C78 C79 112.04(11) . . ?
C74 C78 C80 110.78(11) . . ?
C79 C78 H78 107.7 . . ?
C79 C78 C80 110.74(11) . . ?
C80 C78 H78 107.7 . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 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
O2 C8 C9 C10 168.00(10) . . . . ?
O2 C8 C9 C14 -8.93(17) . . . . ?
O2 C8 C13 C12 -168.06(10) . . . . ?
O2 C8 C13 C16 9.85(16) . . . . ?
N1 C2 C6 C7 11.7(2) . . . . ?
N1 C17 C18 C19 -176.87(10) . . . . ?
N1 C17 C18 C23 6.92(16) . . . . ?
N1 C17 C22 C21 177.57(10) . . . . ?
N1 C17 C22 C26 -0.99(16) . . . . ?
N2 C2 C6 C7 -169.96(11) . . . . ?
N2 C4 C5 N1 0.60(12) . . . . ?
N2 C29 C30 C31 -179.51(10) . . . . ?
N2 C29 C30 C35 0.60(16) . . . . ?
N2 C29 C34 C33 179.59(10) . . . . ?
N2 C29 C34 C38 -1.92(16) . . . . ?
C2 N1 C5 C4 -0.24(13) . . . . ?
C2 N1 C17 C18 -110.66(13) . . . . ?
C2 N1 C17 C22 71.46(15) . . . . ?
C2 N2 C4 C5 -0.76(13) . . . . ?
C2 N2 C29 C30 -86.37(13) . . . . ?
C2 N2 C29 C34 92.50(13) . . . . ?
C2 C6 C7 O1 -1.6(2) . . . . ?
C2 C6 C7 O2 177.53(11) . . . . ?
C4 N2 C2 N1 0.60(12) . . . . ?
C4 N2 C2 C6 -178.12(10) . . . . ?
C4 N2 C29 C30 71.11(14) . . . . ?
C4 N2 C29 C34 -110.02(12) . . . . ?
C5 N1 C2 N2 -0.23(12) . . . . ?
C5 N1 C2 C6 178.29(12) . . . . ?
C5 N1 C17 C18 71.59(14) . . . . ?
C5 N1 C17 C22 -106.28(12) . . . . ?
C7 O2 C8 C9 66.09(15) . . . . ?
C7 O2 C8 C13 -122.99(11) . . . . ?
C8 O2 C7 O1 14.10(17) . . . . ?
C8 O2 C7 C6 -165.20(10) . . . . ?
C8 C9 C10 C11 -0.44(18) . . . . ?
C9 C8 C13 C12 2.74(17) . . . . ?
C9 C8 C13 C16 -179.35(11) . . . . ?
C9 C10 C11 C12 2.77(18) . . . . ?
C9 C10 C11 C15 -175.46(11) . . . . ?
C10 C11 C12 C13 -2.41(17) . . . . ?
C11 C12 C13 C8 -0.25(17) . . . . ?
C11 C12 C13 C16 -178.14(12) . . . . ?
C13 C8 C9 C10 -2.40(17) . . . . ?
C13 C8 C9 C14 -179.33(11) . . . . ?
C14 C9 C10 C11 176.54(12) . . . . ?
C15 C11 C12 C13 175.83(11) . . . . ?
C17 N1 C2 N2 -178.19(10) . . . . ?
C17 N1 C2 C6 0.3(2) . . . . ?
C17 N1 C5 C4 177.89(10) . . . . ?
C17 C18 C19 C20 -0.73(18) . . . . ?
C17 C18 C23 C24 94.56(14) . . . . ?
C17 C18 C23 C25 -140.48(12) . . . . ?
C17 C22 C26 C27 -149.66(12) . . . . ?
C17 C22 C26 C28 85.63(14) . . . . ?
C18 C17 C22 C21 -0.17(17) . . . . ?
C18 C17 C22 C26 -178.72(11) . . . . ?
C18 C19 C20 C21 -0.1(2) . . . . ?
C19 C18 C23 C24 -81.49(15) . . . . ?
C19 C18 C23 C25 43.47(17) . . . . ?
C19 C20 C21 C22 0.9(2) . . . . ?
C20 C21 C22 C17 -0.74(18) . . . . ?
C20 C21 C22 C26 177.80(12) . . . . ?
C21 C22 C26 C27 31.87(17) . . . . ?
C21 C22 C26 C28 -92.84(14) . . . . ?
C22 C17 C18 C19 0.89(17) . . . . ?
C22 C17 C18 C23 -175.32(11) . . . . ?
C23 C18 C19 C20 175.49(12) . . . . ?
C29 N2 C2 N1 160.84(10) . . . . ?
C29 N2 C2 C6 -17.88(16) . . . . ?
C29 N2 C4 C5 -160.79(10) . . . . ?
C29 C30 C31 C32 -0.75(18) . . . . ?
C29 C30 C35 C36 138.99(12) . . . . ?
C29 C30 C35 C37 -96.50(13) . . . . ?
C29 C34 C38 C39 -111.47(13) . . . . ?
C29 C34 C38 C40 125.46(12) . . . . ?
C30 C29 C34 C33 -1.61(16) . . . . ?
C30 C29 C34 C38 176.88(11) . . . . ?
C30 C31 C32 C33 -0.1(2) . . . . ?
C31 C30 C35 C36 -40.90(16) . . . . ?
C31 C30 C35 C37 83.61(14) . . . . ?
C31 C32 C33 C34 0.2(2) . . . . ?
C32 C33 C34 C29 0.67(18) . . . . ?
C32 C33 C34 C38 -177.85(11) . . . . ?
C33 C34 C38 C39 66.97(15) . . . . ?
C33 C34 C38 C40 -56.10(15) . . . . ?
C34 C29 C30 C31 1.66(17) . . . . ?
C34 C29 C30 C35 -178.23(10) . . . . ?
C35 C30 C31 C32 179.14(12) . . . . ?
O4 C48 C49 C50 -176.16(10) . . . . ?
O4 C48 C49 C54 4.81(17) . . . . ?
O4 C48 C53 C52 177.07(10) . . . . ?
O4 C48 C53 C56 -3.07(18) . . . . ?
N3 C42 C46 C47 163.02(12) . . . . ?
N3 C57 C58 C59 174.19(10) . . . . ?
N3 C57 C58 C63 -4.67(16) . . . . ?
N3 C57 C62 C61 -174.43(10) . . . . ?
N3 C57 C62 C66 5.24(17) . . . . ?
N4 C42 C46 C47 -17.6(2) . . . . ?
N4 C44 C45 N3 -0.14(13) . . . . ?
N4 C69 C70 C71 177.19(10) . . . . ?
N4 C69 C70 C75 -3.15(16) . . . . ?
N4 C69 C74 C73 -177.59(10) . . . . ?
N4 C69 C74 C78 3.17(17) . . . . ?
C42 N3 C45 C44 0.53(13) . . . . ?
C42 N3 C57 C58 -78.95(14) . . . . ?
C42 N3 C57 C62 97.35(13) . . . . ?
C42 N4 C44 C45 -0.29(14) . . . . ?
C42 N4 C69 C70 100.61(14) . . . . ?
C42 N4 C69 C74 -82.49(15) . . . . ?
C42 C46 C47 O3 5.7(2) . . . . ?
C42 C46 C47 O4 -172.46(12) . . . . ?
C44 N4 C42 N3 0.59(12) . . . . ?
C44 N4 C42 C46 -178.84(12) . . . . ?
C44 N4 C69 C70 -88.97(14) . . . . ?
C44 N4 C69 C74 87.93(14) . . . . ?
C45 N3 C42 N4 -0.69(12) . . . . ?
C45 N3 C42 C46 178.82(10) . . . . ?
C45 N3 C57 C58 95.52(14) . . . . ?
C45 N3 C57 C62 -88.18(14) . . . . ?
C47 O4 C48 C49 -101.57(13) . . . . ?
C47 O4 C48 C53 82.69(14) . . . . ?
C48 O4 C47 O3 -0.95(18) . . . . ?
C48 O4 C47 C46 177.45(11) . . . . ?
C48 C49 C50 C51 -0.92(18) . . . . ?
C49 C48 C53 C52 1.52(18) . . . . ?
C49 C48 C53 C56 -178.62(12) . . . . ?
C49 C50 C51 C52 1.31(18) . . . . ?
C49 C50 C51 C55 -178.18(12) . . . . ?
C50 C51 C52 C53 -0.27(19) . . . . ?
C51 C52 C53 C48 -1.11(19) . . . . ?
C51 C52 C53 C56 179.04(13) . . . . ?
C53 C48 C49 C50 -0.55(18) . . . . ?
C53 C48 C49 C54 -179.58(12) . . . . ?
C54 C49 C50 C51 178.11(12) . . . . ?
C55 C51 C52 C53 179.22(12) . . . . ?
C57 N3 C42 N4 174.59(9) . . . . ?
C57 N3 C42 C46 -5.90(16) . . . . ?
C57 N3 C45 C44 -174.52(11) . . . . ?
C57 C58 C59 C60 0.19(17) . . . . ?
C57 C58 C63 C64 -127.86(12) . . . . ?
C57 C58 C63 C65 109.37(13) . . . . ?
C57 C62 C66 C67 113.36(15) . . . . ?
C57 C62 C66 C68 -122.09(16) . . . . ?
C58 C57 C62 C61 1.69(17) . . . . ?
C58 C57 C62 C66 -178.65(11) . . . . ?
C58 C59 C60 C61 1.74(19) . . . . ?
C59 C58 C63 C64 53.32(15) . . . . ?
C59 C58 C63 C65 -69.45(14) . . . . ?
C59 C60 C61 C62 -2.00(19) . . . . ?
C60 C61 C62 C57 0.32(18) . . . . ?
C60 C61 C62 C66 -179.35(12) . . . . ?
C61 C62 C66 C67 -66.99(18) . . . . ?
C61 C62 C66 C68 57.56(19) . . . . ?
C62 C57 C58 C59 -1.93(17) . . . . ?
C62 C57 C58 C63 179.20(11) . . . . ?
C63 C58 C59 C60 179.08(11) . . . . ?
C69 N4 C42 N3 171.93(10) . . . . ?
C69 N4 C42 C46 -7.5(2) . . . . ?
C69 N4 C44 C45 -172.33(10) . . . . ?
C69 C70 C71 C72 0.12(18) . . . . ?
C69 C70 C75 C76 -126.04(13) . . . . ?
C69 C70 C75 C77 110.79(13) . . . . ?
C69 C74 C78 C79 -131.13(12) . . . . ?
C69 C74 C78 C80 104.65(13) . . . . ?
C70 C69 C74 C73 -0.85(17) . . . . ?
C70 C69 C74 C78 179.91(11) . . . . ?
C70 C71 C72 C73 -0.3(2) . . . . ?
C71 C70 C75 C76 53.60(16) . . . . ?
C71 C70 C75 C77 -69.57(15) . . . . ?
C71 C72 C73 C74 -0.1(2) . . . . ?
C72 C73 C74 C69 0.67(18) . . . . ?
C72 C73 C74 C78 179.92(12) . . . . ?
C73 C74 C78 C79 49.66(16) . . . . ?
C73 C74 C78 C80 -74.56(15) . . . . ?
C74 C69 C70 C71 0.47(17) . . . . ?
C74 C69 C70 C75 -179.88(11) . . . . ?
C75 C70 C71 C72 -179.54(12) . . . . ?

_olex2_date_sample_data_collection 2021-05-04
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.730
####################################################################### 
# 
# 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_wf458
_database_code_depnum_ccdc_archive 'CCDC 2097046'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-16 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-07-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H24 N2 O'
_chemical_formula_sum            'C23 H24 N2 O'
_chemical_formula_weight         344.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C23 H24 N2 O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   9.28771(11)
_cell_length_b                   13.5951(2)
_cell_length_c                   15.3562(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.7900(15)
_cell_angle_gamma                90
_cell_volume                     1938.80(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14883
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.6300
_cell_measurement_theta_min      4.3300
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.925
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             736
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0563
0 -1 1 0.0233
0 1 -1 0.0308
-1 -2 -2 0.0397
1 2 2 0.0256
-1 1 2 0.0600
1 -1 -2 0.0602
1 1 2 0.0214
-1 -1 -2 0.0308
0 0 1 0.0342

_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
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
1.0000 0.0000 -0.0000 -0.0548 -0.0546 0.1467
0.0000 -1.0000 1.0000 -0.1411 0.0416 -0.0356
-0.0000 1.0000 -1.0000 0.1411 -0.0416 0.0356
-1.0000 -2.0000 -2.0000 -0.0282 -0.2055 -0.2773
1.0000 2.0000 2.0000 0.0282 0.2055 0.2773
-1.0000 1.0000 2.0000 0.0465 0.2706 -0.0665
1.0000 -1.0000 -2.0000 -0.0465 -0.2706 0.0665
1.0000 1.0000 2.0000 -0.0631 0.1613 0.2269
-1.0000 -1.0000 -2.0000 0.0631 -0.1613 -0.2269
-0.0000 0.0000 1.0000 -0.0498 0.0858 0.0149

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40503
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.060
_diffrn_reflns_theta_min         4.344
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  86.00   0.50    1.00    --   59.26-117.00-103.00  146
  2  ω     72.00  97.00   0.50    1.00    --   59.26-164.00 107.00   50
  3  ω    -82.00 -54.00   0.50    1.00    --  -62.07-164.00 107.00   56
  4  ω    -96.00 -71.00   0.50    1.00    --  -62.07 164.00 132.00   50
  5  ω    -56.00 -16.00   0.50    1.00    --  -62.07 117.00 -16.00   80
  6  ω     51.00  96.00   0.50    1.00    --   73.26-117.00-103.00   90
  7  ω     57.00  82.00   0.50    1.00    --   73.26 164.00 132.00   50
  8  ω   -104.00 -79.00   0.50    2.00    --  -74.55-164.00 107.00   50
  9  ω   -105.00 -80.00   0.50    2.00    --  -75.95-164.00 107.00   50
 10  ω   -106.00 -81.00   0.50    2.00    --  -75.95 164.00 132.00   50
 11  ω    -91.00 -66.00   0.50    2.00    --  -75.95 117.00 -16.00   50
 12  ω     62.00  88.00   0.50    2.00    --   79.85-117.00-103.00   52
 13  ω     61.00  86.00   0.50    2.00    --   79.85-164.00 107.00   50
 14  ω     61.00  86.00   0.50    2.00    --   79.85 164.00 132.00   50
 15  ω     48.00  74.00   0.50    1.00    --   38.00  64.00-171.44   52
 16  ω     44.00  77.00   0.50    1.00    --   38.00  70.00   1.91   66
 17  ω     61.00  94.00   0.50    1.00    --   54.00  68.00 -82.41   66
 18  ω     70.00  99.00   0.50    1.00    --   58.00  69.00-177.03   58
 19  ω   -110.00 -84.00   0.50    1.00    --  -66.00 -57.00 -58.55   52
 20  ω     64.00 115.00   0.50    1.00    --   66.26  28.00 110.00  102
 21  ω     35.00  79.00   0.50    1.00    --   73.26 -95.00 120.00   88
 22  ω   -108.00 -78.00   0.50    1.00    --  -74.00 -74.00  -3.69   60
 23  ω   -127.00 -96.00   0.50    2.00    --  -79.25 -40.00-122.55   62
 24  ω   -119.00 -94.00   0.50    2.00    --  -79.25 -54.00 -28.64   50
 25  ω   -116.00 -91.00   0.50    2.00    --  -79.25 -79.00-170.66   50
 26  ω   -117.00 -84.00   0.50    2.00    --  -79.25 -70.00 142.90   66
 27  ω   -116.00 -81.00   0.50    2.00    --  -79.25 -85.00 -59.10   70
 28  ω   -104.00 -50.00   0.50    2.00    --  -79.25 114.00 -41.58  108
 29  ω     50.00  86.00   0.50    2.00    --   79.85 -95.00   0.00   72
 30  ω     48.00  82.00   0.50    2.00    --   79.85  15.00 -60.00   68
 31  ω     42.00  84.00   0.50    2.00    --   79.85 -95.00 -90.00   84
 32  ω     44.00  81.00   0.50    2.00    --   79.85 -95.00 120.00   74
 33  ω     77.00 103.00   0.50    2.00    --   79.85-111.00 150.00   52
 34  ω     37.00  63.00   0.50    2.00    --   79.85-111.00 -60.00   52
 35  ω     98.00 129.00   0.50    2.00    --   79.85  30.00 -30.00   62
 36  ω     41.00  74.00   0.50    2.00    --   79.85 -95.00  30.00   66
 37  ω     52.00 100.00   0.50    2.00    --   79.85 178.00-150.00   96
 38  ω     61.00 120.00   0.50    2.00    --   79.85 178.00 150.00  118
 39  ω     75.00 101.00   0.50    2.00    --   79.85-111.00 -90.00   52
 40  ω     46.00  97.00   0.50    2.00    --   79.85   0.00-120.00  102
 41  ω     56.00 103.00   0.50    2.00    --   79.85-111.00-150.00   94
 42  ω     84.00 128.00   0.50    2.00    --   79.85  30.00  30.00   88
 43  ω     45.00  70.00   0.50    2.00    --   79.85 -95.00 -60.00   50
 44  ω     35.00  68.00   0.50    2.00    --   79.85-111.00-180.00   66
 45  ω     45.00  79.00   0.50    2.00    --   79.85 -95.00 -30.00   68
 46  ω     73.00  99.00   0.50    2.00    --   79.85-111.00   0.00   52
 47  ω     84.00 113.00   0.50    2.00    --   79.85  30.00  90.00   58
 48  ω     78.00 103.00   0.50    2.00    --   79.85-111.00 120.00   50
 49  ω     37.00  63.00   0.50    2.00    --   79.85-111.00 120.00   52
 50  ω    100.00 127.00   0.50    2.00    --   79.85  30.00-150.00   54
 51  ω     77.00 103.00   0.50    2.00    --   79.85-111.00  30.00   52
 52  ω     47.00  78.00   0.50    2.00    --   79.85 -95.00-150.00   62
 53  ω     35.00  70.00   0.50    2.00    --   79.85-111.00  30.00   70
 54  ω     77.00 103.00   0.50    2.00    --   79.85-111.00-180.00   52
 55  ω     44.00  69.00   0.50    2.00    --   79.85 -95.00 150.00   50
 56  ω     54.00  97.00   0.50    2.00    --   79.85   0.00 -60.00   86
 57  ω     50.00  76.00   0.50    2.00    --   79.85-111.00-120.00   52
 58  ω     70.00  96.00   0.50    2.00    --   79.85-111.00  60.00   52
 59  ω     44.00  74.00   0.50    2.00    --   79.85 -95.00-180.00   60
 60  ω     66.00  96.00   0.50    2.00    --   79.85 178.00  90.00   60
 61  ω     76.00 112.00   0.50    2.00    --   79.85  15.00  90.00   72
 62  ω     53.00 116.00   0.50    2.00    --   79.85 178.00  60.00  126
 63  ω     83.00 108.00   0.50    2.00    --   79.85  30.00-120.00   50
 64  ω     40.00 119.00   0.50    2.00    --   83.00-135.00 -65.07  158
 65  ω     71.00 118.00   0.50    2.00    --   83.00   7.00 -21.97   94
 66  ω     51.00 109.00   0.50    2.00    --   83.00-115.00 -28.68  116
 67  ω     62.00 118.00   0.50    2.00    --   83.00 152.00-153.53  112
 68  ω     86.00 120.00   0.50    2.00    --   83.00  73.00 116.10   68
 69  ω     41.00 122.00   0.50    2.00    --   83.00-140.00 137.65  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0548052000
_diffrn_orient_matrix_UB_12      0.0913008000
_diffrn_orient_matrix_UB_13      -0.0498103000
_diffrn_orient_matrix_UB_21      -0.0546432000
_diffrn_orient_matrix_UB_22      0.0442433000
_diffrn_orient_matrix_UB_23      0.0858419000
_diffrn_orient_matrix_UB_31      0.1467060000
_diffrn_orient_matrix_UB_32      0.0504419000
_diffrn_orient_matrix_UB_33      0.0148729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3238
_reflns_number_total             3989
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.029
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0564P)²+0.3077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1086
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(1)
 Sof(H24D)=Sof(H24E)=Sof(H24F)=FVAR(1)
 Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(3)
 Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(3)
 Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(4)
 Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(4)
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(5)
 Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(5)
 Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(6)
 Sof(H16B)=Sof(H16A)=Sof(H16C)=FVAR(6)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C12(H12), C19(H19), C21(H21)
3.b Disordered Me refined as rotating group:
 C14(H14A,H14B,H14C,H14D,H14E,H14F), C15(H15A,H15B,H15C,H15D,H15E,H15F),
 C16(H16B,H16A,H16C,H16D,H16E,H16F), C23(H23A,H23B,H23C,H23D,H23E,H23F),
 C24(H24A,H24B,H24C,H24D,H24E,H24F), C25(H25A,H25B,H25C,H25D,H25E,H25F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.15916(13) 0.40423(9) 0.23961(10) 0.0903(4) Uani 1 1 d . . . . .
N1 N 0.54203(11) 0.63798(7) 0.28313(7) 0.0444(2) Uani 1 1 d . . . . .
N2 N 0.35759(11) 0.67630(7) 0.20195(7) 0.0434(2) Uani 1 1 d . . . . .
C2 C 0.41602(13) 0.60165(9) 0.25013(8) 0.0416(3) Uani 1 1 d . . . . .
C4 C 0.44667(14) 0.75841(9) 0.20669(9) 0.0484(3) Uani 1 1 d . . . . .
H4 H 0.429712 0.820122 0.179404 0.058 Uiso 1 1 calc R U . . .
C5 C 0.56051(14) 0.73470(9) 0.25664(9) 0.0489(3) Uani 1 1 d . . . . .
H5 H 0.639374 0.776313 0.271273 0.059 Uiso 1 1 calc R U . . .
C6 C 0.36343(13) 0.50863(9) 0.26450(8) 0.0445(3) Uani 1 1 d . . . . .
C7 C 0.25027(15) 0.46425(11) 0.24834(10) 0.0573(3) Uani 1 1 d . . . . .
C8 C 0.63438(12) 0.58295(9) 0.34113(8) 0.0424(3) Uani 1 1 d . . . . .
C9 C 0.73278(13) 0.51702(9) 0.30628(8) 0.0448(3) Uani 1 1 d . . . . .
C10 C 0.81495(13) 0.46169(9) 0.36426(9) 0.0487(3) Uani 1 1 d . . . . .
H10 H 0.884212 0.417108 0.342148 0.058 Uiso 1 1 calc R U . . .
C11 C 0.79885(14) 0.46961(10) 0.45368(9) 0.0500(3) Uani 1 1 d . . . . .
C12 C 0.70182(15) 0.53777(10) 0.48544(9) 0.0523(3) Uani 1 1 d . . . . .
H12 H 0.692302 0.544972 0.546630 0.063 Uiso 1 1 calc R U . . .
C13 C 0.61815(13) 0.59579(9) 0.43020(9) 0.0473(3) Uani 1 1 d . . . . .
C14 C 0.74623(17) 0.50336(11) 0.20984(9) 0.0603(4) Uani 1 1 d . . . . .
H14A H 0.673712 0.456104 0.189268 0.072 Uiso 0.852(15) 1 calc R U P . .
H14B H 0.842589 0.478482 0.196797 0.072 Uiso 0.852(15) 1 calc R U P . .
H14C H 0.731184 0.566578 0.180425 0.072 Uiso 0.852(15) 1 calc R U P . .
H14D H 0.824612 0.544672 0.188392 0.072 Uiso 0.148(15) 1 calc R U P . .
H14E H 0.655734 0.522294 0.180863 0.072 Uiso 0.148(15) 1 calc R U P . .
H14F H 0.767139 0.434198 0.197235 0.072 Uiso 0.148(15) 1 calc R U P . .
C15 C 0.88343(16) 0.40439(11) 0.51476(11) 0.0625(4) Uani 1 1 d . . . . .
H15A H 0.838415 0.339255 0.516822 0.075 Uiso 0.874(16) 1 calc R U P . .
H15B H 0.884651 0.433377 0.573200 0.075 Uiso 0.874(16) 1 calc R U P . .
H15C H 0.982342 0.398060 0.494061 0.075 Uiso 0.874(16) 1 calc R U P . .
H15D H 0.965190 0.441206 0.539234 0.075 Uiso 0.126(16) 1 calc R U P . .
H15E H 0.918954 0.347084 0.482855 0.075 Uiso 0.126(16) 1 calc R U P . .
H15F H 0.821263 0.382401 0.561994 0.075 Uiso 0.126(16) 1 calc R U P . .
C16 C 0.51261(17) 0.66930(12) 0.46480(10) 0.0625(4) Uani 1 1 d . . . . .
H16B H 0.415634 0.653214 0.443242 0.075 Uiso 0.827(17) 1 calc R U P . .
H16A H 0.539039 0.735369 0.445127 0.075 Uiso 0.827(17) 1 calc R U P . .
H16C H 0.514298 0.667266 0.528596 0.075 Uiso 0.827(17) 1 calc R U P . .
H16D H 0.563680 0.717352 0.501401 0.075 Uiso 0.173(17) 1 calc R U P . .
H16E H 0.440275 0.635197 0.499516 0.075 Uiso 0.173(17) 1 calc R U P . .
H16F H 0.465016 0.703300 0.416047 0.075 Uiso 0.173(17) 1 calc R U P . .
C17 C 0.22647(13) 0.66935(8) 0.15142(8) 0.0421(3) Uani 1 1 d . . . . .
C18 C 0.09859(14) 0.70400(9) 0.18719(9) 0.0470(3) Uani 1 1 d . . . . .
C19 C -0.02371(14) 0.70216(10) 0.13439(9) 0.0517(3) Uani 1 1 d . . . . .
H19 H -0.111218 0.727593 0.156459 0.062 Uiso 1 1 calc R U . . .
C20 C -0.02269(14) 0.66445(10) 0.05046(9) 0.0519(3) Uani 1 1 d . . . . .
C21 C 0.10543(14) 0.62619(10) 0.01920(9) 0.0503(3) Uani 1 1 d . . . . .
H21 H 0.106475 0.597719 -0.037289 0.060 Uiso 1 1 calc R U . . .
C22 C 0.23196(13) 0.62853(9) 0.06845(8) 0.0453(3) Uani 1 1 d . . . . .
C23 C 0.09299(17) 0.73942(12) 0.27977(9) 0.0611(4) Uani 1 1 d . . . . .
H23A H 0.076832 0.683366 0.318555 0.073 Uiso 0.671(16) 1 calc R U P . .
H23B H 0.014105 0.786731 0.285667 0.073 Uiso 0.671(16) 1 calc R U P . .
H23C H 0.184370 0.771272 0.295484 0.073 Uiso 0.671(16) 1 calc R U P . .
H23D H 0.106706 0.810880 0.281249 0.073 Uiso 0.329(16) 1 calc R U P . .
H23E H 0.169433 0.707515 0.314137 0.073 Uiso 0.329(16) 1 calc R U P . .
H23F H -0.000832 0.722974 0.304320 0.073 Uiso 0.329(16) 1 calc R U P . .
C24 C -0.15592(16) 0.66609(13) -0.00629(12) 0.0690(4) Uani 1 1 d . . . . .
H24A H -0.129426 0.681294 -0.066358 0.083 Uiso 0.279(18) 1 calc R U P . .
H24B H -0.222244 0.716453 0.014971 0.083 Uiso 0.279(18) 1 calc R U P . .
H24C H -0.202902 0.601595 -0.004461 0.083 Uiso 0.279(18) 1 calc R U P . .
H24D H -0.240289 0.651600 0.029126 0.083 Uiso 0.721(18) 1 calc R U P . .
H24E H -0.147471 0.616442 -0.052203 0.083 Uiso 0.721(18) 1 calc R U P . .
H24F H -0.166813 0.731300 -0.032771 0.083 Uiso 0.721(18) 1 calc R U P . .
C25 C 0.36930(15) 0.58556(11) 0.03448(9) 0.0544(3) Uani 1 1 d . . . . .
H25A H 0.448587 0.631837 0.044877 0.065 Uiso 0.842(15) 1 calc R U P . .
H25B H 0.358797 0.573326 -0.028181 0.065 Uiso 0.842(15) 1 calc R U P . .
H25C H 0.390058 0.523496 0.064584 0.065 Uiso 0.842(15) 1 calc R U P . .
H25D H 0.349708 0.520602 0.009309 0.065 Uiso 0.158(15) 1 calc R U P . .
H25E H 0.439498 0.579114 0.082367 0.065 Uiso 0.158(15) 1 calc R U P . .
H25F H 0.408237 0.628944 -0.010397 0.065 Uiso 0.158(15) 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.1818(17) . ?
N1 C2 1.3616(15) . ?
N1 C5 1.3877(16) . ?
N1 C8 1.4379(15) . ?
N2 C2 1.3641(15) . ?
N2 C4 1.3908(16) . ?
N2 C17 1.4381(15) . ?
C2 C6 1.3745(17) . ?
C4 H4 0.9500 . ?
C4 C5 1.3371(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.2341(18) . ?
C8 C9 1.3924(18) . ?
C8 C13 1.3891(18) . ?
C9 C10 1.3865(17) . ?
C9 C14 1.4994(19) . ?
C10 H10 0.9500 . ?
C10 C11 1.3875(19) . ?
C11 C12 1.386(2) . ?
C11 C15 1.5043(18) . ?
C12 H12 0.9500 . ?
C12 C13 1.3884(18) . ?
C13 C16 1.5021(19) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 H14D 0.9800 . ?
C14 H14E 0.9800 . ?
C14 H14F 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15D 0.9800 . ?
C15 H15E 0.9800 . ?
C15 H15F 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16C 0.9800 . ?
C16 H16D 0.9800 . ?
C16 H16E 0.9800 . ?
C16 H16F 0.9800 . ?
C17 C18 1.3972(17) . ?
C17 C22 1.3914(17) . ?
C18 C19 1.3866(18) . ?
C18 C23 1.5027(19) . ?
C19 H19 0.9500 . ?
C19 C20 1.387(2) . ?
C20 C21 1.3903(19) . ?
C20 C24 1.5037(19) . ?
C21 H21 0.9500 . ?
C21 C22 1.3891(17) . ?
C22 C25 1.5029(18) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 H23D 0.9800 . ?
C23 H23E 0.9800 . ?
C23 H23F 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 H25D 0.9800 . ?
C25 H25E 0.9800 . ?
C25 H25F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C5 110.11(10) . . ?
C2 N1 C8 122.96(10) . . ?
C5 N1 C8 126.82(10) . . ?
C2 N2 C4 109.69(10) . . ?
C2 N2 C17 124.85(10) . . ?
C4 N2 C17 125.42(10) . . ?
N1 C2 N2 105.39(10) . . ?
N1 C2 C6 125.42(11) . . ?
N2 C2 C6 129.19(11) . . ?
N2 C4 H4 126.2 . . ?
C5 C4 N2 107.55(11) . . ?
C5 C4 H4 126.2 . . ?
N1 C5 H5 126.4 . . ?
C4 C5 N1 107.25(11) . . ?
C4 C5 H5 126.4 . . ?
C7 C6 C2 136.14(13) . . ?
O1 C7 C6 165.20(17) . . ?
C9 C8 N1 119.07(11) . . ?
C13 C8 N1 118.21(11) . . ?
C13 C8 C9 122.69(11) . . ?
C8 C9 C14 121.56(12) . . ?
C10 C9 C8 117.44(12) . . ?
C10 C9 C14 120.96(12) . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 121.84(12) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C15 120.59(13) . . ?
C12 C11 C10 118.67(12) . . ?
C12 C11 C15 120.74(13) . . ?
C11 C12 H12 119.1 . . ?
C11 C12 C13 121.73(13) . . ?
C13 C12 H12 119.1 . . ?
C8 C13 C16 120.80(12) . . ?
C12 C13 C8 117.57(12) . . ?
C12 C13 C16 121.62(13) . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
C9 C14 H14D 109.5 . . ?
C9 C14 H14E 109.5 . . ?
C9 C14 H14F 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14A C14 H14D 141.1 . . ?
H14A C14 H14E 56.3 . . ?
H14A C14 H14F 56.3 . . ?
H14B C14 H14C 109.5 . . ?
H14B C14 H14D 56.3 . . ?
H14B C14 H14E 141.1 . . ?
H14B C14 H14F 56.3 . . ?
H14C C14 H14D 56.3 . . ?
H14C C14 H14E 56.3 . . ?
H14C C14 H14F 141.1 . . ?
H14D C14 H14E 109.5 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
C11 C15 H15D 109.5 . . ?
C11 C15 H15E 109.5 . . ?
C11 C15 H15F 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15A C15 H15D 141.1 . . ?
H15A C15 H15E 56.3 . . ?
H15A C15 H15F 56.3 . . ?
H15B C15 H15C 109.5 . . ?
H15B C15 H15D 56.3 . . ?
H15B C15 H15E 141.1 . . ?
H15B C15 H15F 56.3 . . ?
H15C C15 H15D 56.3 . . ?
H15C C15 H15E 56.3 . . ?
H15C C15 H15F 141.1 . . ?
H15D C15 H15E 109.5 . . ?
H15D C15 H15F 109.5 . . ?
H15E C15 H15F 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16C 109.5 . . ?
C13 C16 H16D 109.5 . . ?
C13 C16 H16E 109.5 . . ?
C13 C16 H16F 109.5 . . ?
H16B C16 H16A 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H16B C16 H16D 141.1 . . ?
H16B C16 H16E 56.3 . . ?
H16B C16 H16F 56.3 . . ?
H16A C16 H16C 109.5 . . ?
H16A C16 H16D 56.3 . . ?
H16A C16 H16E 141.1 . . ?
H16A C16 H16F 56.3 . . ?
H16C C16 H16D 56.3 . . ?
H16C C16 H16E 56.3 . . ?
H16C C16 H16F 141.1 . . ?
H16D C16 H16E 109.5 . . ?
H16D C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?
C18 C17 N2 118.94(11) . . ?
C22 C17 N2 118.61(10) . . ?
C22 C17 C18 122.45(11) . . ?
C17 C18 C23 121.37(12) . . ?
C19 C18 C17 117.26(12) . . ?
C19 C18 C23 121.35(12) . . ?
C18 C19 H19 118.9 . . ?
C18 C19 C20 122.27(12) . . ?
C20 C19 H19 118.9 . . ?
C19 C20 C21 118.42(12) . . ?
C19 C20 C24 121.12(13) . . ?
C21 C20 C24 120.45(14) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.68(13) . . ?
C22 C21 H21 119.2 . . ?
C17 C22 C25 120.99(11) . . ?
C21 C22 C17 117.80(11) . . ?
C21 C22 C25 121.18(12) . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
C18 C23 H23D 109.5 . . ?
C18 C23 H23E 109.5 . . ?
C18 C23 H23F 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23A C23 H23D 141.1 . . ?
H23A C23 H23E 56.3 . . ?
H23A C23 H23F 56.3 . . ?
H23B C23 H23C 109.5 . . ?
H23B C23 H23D 56.3 . . ?
H23B C23 H23E 141.1 . . ?
H23B C23 H23F 56.3 . . ?
H23C C23 H23D 56.3 . . ?
H23C C23 H23E 56.3 . . ?
H23C C23 H23F 141.1 . . ?
H23D C23 H23E 109.5 . . ?
H23D C23 H23F 109.5 . . ?
H23E C23 H23F 109.5 . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.5 . . ?
C20 C24 H24C 109.5 . . ?
C20 C24 H24D 109.5 . . ?
C20 C24 H24E 109.5 . . ?
C20 C24 H24F 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24A C24 H24D 141.1 . . ?
H24A C24 H24E 56.3 . . ?
H24A C24 H24F 56.3 . . ?
H24B C24 H24C 109.5 . . ?
H24B C24 H24D 56.3 . . ?
H24B C24 H24E 141.1 . . ?
H24B C24 H24F 56.3 . . ?
H24C C24 H24D 56.3 . . ?
H24C C24 H24E 56.3 . . ?
H24C C24 H24F 141.1 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
C22 C25 H25D 109.5 . . ?
C22 C25 H25E 109.5 . . ?
C22 C25 H25F 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25A C25 H25D 141.1 . . ?
H25A C25 H25E 56.3 . . ?
H25A C25 H25F 56.3 . . ?
H25B C25 H25C 109.5 . . ?
H25B C25 H25D 56.3 . . ?
H25B C25 H25E 141.1 . . ?
H25B C25 H25F 56.3 . . ?
H25C C25 H25D 56.3 . . ?
H25C C25 H25E 56.3 . . ?
H25C C25 H25F 141.1 . . ?
H25D C25 H25E 109.5 . . ?
H25D C25 H25F 109.5 . . ?
H25E C25 H25F 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 C2 C6 C7 172.26(17) . . . . ?
N1 C8 C9 C10 -176.84(10) . . . . ?
N1 C8 C9 C14 1.00(18) . . . . ?
N1 C8 C13 C12 176.11(11) . . . . ?
N1 C8 C13 C16 -3.32(18) . . . . ?
N2 C2 C6 C7 -7.6(3) . . . . ?
N2 C4 C5 N1 -0.16(15) . . . . ?
N2 C17 C18 C19 175.77(11) . . . . ?
N2 C17 C18 C23 -5.74(18) . . . . ?
N2 C17 C22 C21 -177.36(11) . . . . ?
N2 C17 C22 C25 4.53(18) . . . . ?
C2 N1 C5 C4 -0.42(15) . . . . ?
C2 N1 C8 C9 84.08(15) . . . . ?
C2 N1 C8 C13 -93.92(14) . . . . ?
C2 N2 C4 C5 0.68(15) . . . . ?
C2 N2 C17 C18 97.61(14) . . . . ?
C2 N2 C17 C22 -82.58(15) . . . . ?
C2 C6 C7 O1 172.1(6) . . . . ?
C4 N2 C2 N1 -0.92(14) . . . . ?
C4 N2 C2 C6 178.97(13) . . . . ?
C4 N2 C17 C18 -84.90(15) . . . . ?
C4 N2 C17 C22 94.91(15) . . . . ?
C5 N1 C2 N2 0.82(14) . . . . ?
C5 N1 C2 C6 -179.07(12) . . . . ?
C5 N1 C8 C9 -100.00(15) . . . . ?
C5 N1 C8 C13 82.00(16) . . . . ?
C8 N1 C2 N2 177.35(11) . . . . ?
C8 N1 C2 C6 -2.5(2) . . . . ?
C8 N1 C5 C4 -176.78(12) . . . . ?
C8 C9 C10 C11 1.22(18) . . . . ?
C9 C8 C13 C12 -1.81(18) . . . . ?
C9 C8 C13 C16 178.76(12) . . . . ?
C9 C10 C11 C12 -2.65(19) . . . . ?
C9 C10 C11 C15 176.43(12) . . . . ?
C10 C11 C12 C13 1.9(2) . . . . ?
C11 C12 C13 C8 0.3(2) . . . . ?
C11 C12 C13 C16 179.73(13) . . . . ?
C13 C8 C9 C10 1.07(18) . . . . ?
C13 C8 C9 C14 178.91(12) . . . . ?
C14 C9 C10 C11 -176.64(12) . . . . ?
C15 C11 C12 C13 -177.22(12) . . . . ?
C17 N2 C2 N1 176.91(11) . . . . ?
C17 N2 C2 C6 -3.2(2) . . . . ?
C17 N2 C4 C5 -177.13(11) . . . . ?
C17 C18 C19 C20 2.32(19) . . . . ?
C18 C17 C22 C21 2.44(18) . . . . ?
C18 C17 C22 C25 -175.67(12) . . . . ?
C18 C19 C20 C21 0.9(2) . . . . ?
C18 C19 C20 C24 -178.19(13) . . . . ?
C19 C20 C21 C22 -2.6(2) . . . . ?
C20 C21 C22 C17 0.96(19) . . . . ?
C20 C21 C22 C25 179.07(13) . . . . ?
C22 C17 C18 C19 -4.03(18) . . . . ?
C22 C17 C18 C23 174.46(12) . . . . ?
C23 C18 C19 C20 -176.17(13) . . . . ?
C24 C20 C21 C22 176.49(13) . . . . ?

_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.290
_oxdiff_exptl_absorpt_empirical_full_min 0.806
####################################################################### 
# 
# 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_pv167_final
_database_code_depnum_ccdc_archive 'CCDC 2094730'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-08-10 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-08-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H36 N2 O'
_chemical_formula_sum            'C29 H36 N2 O'
_chemical_formula_weight         428.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   16.8250(4)
_cell_length_b                   8.93762(18)
_cell_length_c                   21.4865(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.212(2)
_cell_angle_gamma                90
_cell_volume                     3069.19(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.3620
_cell_measurement_theta_min      5.3920
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.888
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 5 0 0.0535
-4 -5 0 0.0355
-4 0 14 0.1410
3 0 -14 0.1208
-7 4 2 0.0228
7 -4 -2 0.0209

_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.044
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3163
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.721
_diffrn_reflns_theta_min         4.332
_diffrn_ambient_temperature      140.15
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00 -37.00   1.00   10.00    --  -40.91 108.00 -99.00   25
  2  ω     28.00  55.00   1.00   10.00    --   40.91-108.00 163.00   27
  3  ω     56.00  84.00   1.00   10.00    --   40.91-108.00 163.00   28
  4  ω    117.00 142.00   1.00   40.00    --  105.15 108.00 -99.00   25
  5  ω    -50.00 -18.00   1.00   10.00    --  -40.91 -38.00-120.00   32
  6  ω   -113.00 -54.00   1.00   10.00    --  -40.91 -38.00-120.00   59
  7  ω    -32.00  65.00   1.00   10.00    --   40.91 -38.00  30.00   97
  8  ω     34.00  81.00   1.00   10.00    --   40.91 -99.00  60.00   47
  9  ω     14.00  39.00   1.00   10.00    --   40.91 -99.00   0.00   25
 10  ω     77.00 126.00   1.00   40.00    --  105.15 -45.00   0.00   49
 11  ω    106.00 157.00   1.00   40.00    --  105.15  77.00-150.00   51
 12  ω    108.00 178.00   1.00   40.00    --  105.15  77.00  60.00   70
 13  ω    105.00 178.00   1.00   40.00    --  105.15 111.00-120.00   73
 14  ω    113.00 177.00   1.00   40.00    --  105.15 111.00  30.00   64
 15  ω     76.00 104.00   1.00   40.00    --  105.15 -94.00-150.00   28
 16  ω    105.00 176.00   1.00   40.00    --  105.15 111.00 150.00   71
 17  ω    113.00 175.00   1.00   40.00    --  105.15 111.00 -30.00   62
 18  ω     79.00 106.00   1.00   40.00    --  105.15 -61.00 -60.00   27
 19  ω     75.00 102.00   1.00   40.00    --  105.15-108.00 163.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2346
_reflns_number_total             3163
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         0.130
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3163
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.006
_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)+(0.0653P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1035
_refine_special_details          
;
 Refined as a 3-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.699(6)
 0.163(4) 0.138(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: O1(0.5) C3(0.5) C4(0.5)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C8(H8), C9(H9)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
O1 O 0.27529(17) 0.3028(2) 0.51402(15) 0.0706(9) Uani 0.5 1 d . U P A -1
N1 N 0.31754(6) 0.81167(10) 0.51059(4) 0.0295(2) Uani 1 1 d . . . . .
C1 C 0.29156(7) 0.95979(12) 0.50671(5) 0.0325(2) Uani 1 1 d . . . . .
H1 H 0.326494 1.045531 0.512538 0.039 Uiso 1 1 calc R U . . .
C2 C 0.250000 0.71928(17) 0.500000 0.0294(3) Uani 1 2 d S TU P . .
C3 C 0.2424(7) 0.5665(2) 0.5039(6) 0.0313(14) Uani 0.5 1 d . U P A -1
C4 C 0.2608(6) 0.4348(2) 0.5078(4) 0.0394(11) Uani 0.5 1 d . U P A -1
C5 C 0.40238(7) 0.76158(12) 0.52336(5) 0.0326(2) Uani 1 1 d . . . . .
C6 C 0.43803(8) 0.77082(13) 0.47254(5) 0.0375(3) Uani 1 1 d . . . . .
C7 C 0.52037(9) 0.72357(16) 0.48637(7) 0.0492(3) Uani 1 1 d . . . . .
H7 H 0.546425 0.728309 0.453052 0.059 Uiso 1 1 calc R U . . .
C8 C 0.56520(9) 0.66978(17) 0.54761(7) 0.0542(4) Uani 1 1 d . . . . .
H8 H 0.621419 0.637739 0.556008 0.065 Uiso 1 1 calc R U . . .
C9 C 0.52832(8) 0.66268(16) 0.59642(6) 0.0489(3) Uani 1 1 d . . . . .
H9 H 0.559844 0.626049 0.638376 0.059 Uiso 1 1 calc R U . . .
C10 C 0.44621(7) 0.70774(14) 0.58581(5) 0.0381(3) Uani 1 1 d . . . . .
C11 C 0.38734(8) 0.82562(15) 0.40473(5) 0.0427(3) Uani 1 1 d . . . . .
H11 H 0.343600 0.895432 0.410278 0.051 Uiso 1 1 calc R U . . .
C12 C 0.34227(10) 0.69595(18) 0.36201(6) 0.0574(4) Uani 1 1 d . . . . .
H12A H 0.383558 0.627331 0.354159 0.086 Uiso 1 1 calc R U . . .
H12B H 0.306095 0.734800 0.320065 0.086 Uiso 1 1 calc R U . . .
H12C H 0.308197 0.642395 0.384357 0.086 Uiso 1 1 calc R U . . .
C13 C 0.44037(11) 0.91259(19) 0.37111(7) 0.0627(4) Uani 1 1 d . . . . .
H13A H 0.470417 0.992755 0.400114 0.094 Uiso 1 1 calc R U . . .
H13B H 0.404042 0.956071 0.330232 0.094 Uiso 1 1 calc R U . . .
H13C H 0.480731 0.844846 0.361368 0.094 Uiso 1 1 calc R U . . .
C14 C 0.40738(8) 0.69752(16) 0.64079(5) 0.0438(3) Uani 1 1 d . . . . .
H14 H 0.348024 0.732049 0.623064 0.053 Uiso 1 1 calc R U . . .
C15 C 0.45250(11) 0.8003(2) 0.69802(7) 0.0656(4) Uani 1 1 d . . . . .
H15A H 0.510472 0.766675 0.717277 0.098 Uiso 1 1 calc R U . . .
H15B H 0.423869 0.796715 0.731320 0.098 Uiso 1 1 calc R U . . .
H15C H 0.452009 0.903081 0.682067 0.098 Uiso 1 1 calc R U . . .
C16 C 0.40659(11) 0.53723(19) 0.66410(7) 0.0671(4) Uani 1 1 d . . . . .
H16A H 0.379295 0.472790 0.626609 0.101 Uiso 1 1 calc R U . . .
H16B H 0.375778 0.532340 0.695941 0.101 Uiso 1 1 calc R U . . .
H16C H 0.464197 0.503159 0.684798 0.101 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
O1 C4 1.204(3) . ?
N1 C1 1.3884(14) . ?
N1 C2 1.3651(13) . ?
N1 C5 1.4382(14) . ?
C1 C1 1.337(2) 2_556 ?
C1 H1 0.9500 . ?
C2 C3 1.376(3) . ?
C3 C4 1.201(5) 2_556 ?
C3 C4 1.213(5) . ?
C5 C6 1.4029(16) . ?
C5 C10 1.3991(15) . ?
C6 C7 1.3887(18) . ?
C6 C11 1.5210(16) . ?
C7 H7 0.9500 . ?
C7 C8 1.3824(19) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.3876(18) . ?
C10 C14 1.5209(17) . ?
C11 H11 1.0000 . ?
C11 C12 1.5250(19) . ?
C11 C13 1.5247(19) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14 1.0000 . ?
C14 C15 1.5323(18) . ?
C14 C16 1.519(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C5 125.69(9) . . ?
C2 N1 C1 109.67(9) . . ?
C2 N1 C5 124.64(9) . . ?
N1 C1 H1 126.2 . . ?
C1 C1 N1 107.55(6) 2_556 . ?
C1 C1 H1 126.2 2_556 . ?
N1 C2 N1 105.56(13) . 2_556 ?
N1 C2 C3 132.7(5) . . ?
N1 C2 C3 121.5(5) 2_556 . ?
C4 C3 C2 163.5(12) 2_556 . ?
C4 C3 C2 160.1(12) . . ?
C4 C3 C4 19.5(5) 2_556 . ?
O1 C4 C3 175.5(13) . . ?
C6 C5 N1 118.26(9) . . ?
C10 C5 N1 118.96(9) . . ?
C10 C5 C6 122.78(11) . . ?
C5 C6 C11 121.10(10) . . ?
C7 C6 C5 117.14(10) . . ?
C7 C6 C11 121.74(10) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 C6 121.36(12) . . ?
C8 C7 H7 119.3 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 119.95(12) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.2 . . ?
C8 C9 C10 121.61(11) . . ?
C10 C9 H9 119.2 . . ?
C5 C10 C14 122.68(11) . . ?
C9 C10 C5 117.17(11) . . ?
C9 C10 C14 120.15(10) . . ?
C6 C11 H11 107.5 . . ?
C6 C11 C12 110.87(11) . . ?
C6 C11 C13 112.47(12) . . ?
C12 C11 H11 107.5 . . ?
C13 C11 H11 107.5 . . ?
C13 C11 C12 110.90(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14 107.8 . . ?
C10 C14 C15 111.23(11) . . ?
C15 C14 H14 107.8 . . ?
C16 C14 C10 111.28(12) . . ?
C16 C14 H14 107.8 . . ?
C16 C14 C15 110.71(11) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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 C2 C3 C4 -79(4) . . . 2_556 ?
N1 C2 C3 C4 173(3) 2_556 . . . ?
N1 C2 C3 C4 108(3) 2_556 . . 2_556 ?
N1 C2 C3 C4 -14(4) . . . . ?
N1 C5 C6 C7 179.18(11) . . . . ?
N1 C5 C6 C11 -2.74(17) . . . . ?
N1 C5 C10 C9 -179.02(11) . . . . ?
N1 C5 C10 C14 0.99(17) . . . . ?
C1 N1 C2 N1 0.18(5) . . . 2_556 ?
C1 N1 C2 C3 -173.7(7) . . . . ?
C1 N1 C5 C6 -75.77(13) . . . . ?
C1 N1 C5 C10 103.41(13) . . . . ?
C2 N1 C1 C1 -0.49(13) . . . 2_556 ?
C2 N1 C5 C6 103.80(11) . . . . ?
C2 N1 C5 C10 -77.03(12) . . . . ?
C5 N1 C1 C1 179.13(10) . . . 2_556 ?
C5 N1 C2 N1 -179.45(10) . . . 2_556 ?
C5 N1 C2 C3 6.7(7) . . . . ?
C5 C6 C7 C8 0.0(2) . . . . ?
C5 C6 C11 C12 -89.04(14) . . . . ?
C5 C6 C11 C13 146.15(12) . . . . ?
C5 C10 C14 C15 -116.37(14) . . . . ?
C5 C10 C14 C16 119.68(14) . . . . ?
C6 C5 C10 C9 0.11(18) . . . . ?
C6 C5 C10 C14 -179.87(11) . . . . ?
C6 C7 C8 C9 -0.2(2) . . . . ?
C7 C6 C11 C12 88.95(16) . . . . ?
C7 C6 C11 C13 -35.86(18) . . . . ?
C7 C8 C9 C10 0.4(2) . . . . ?
C8 C9 C10 C5 -0.3(2) . . . . ?
C8 C9 C10 C14 179.67(13) . . . . ?
C9 C10 C14 C15 63.65(17) . . . . ?
C9 C10 C14 C16 -60.30(16) . . . . ?
C10 C5 C6 C7 0.04(18) . . . . ?
C10 C5 C6 C11 178.12(11) . . . . ?
C11 C6 C7 C8 -178.07(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.699(6)
2 0.163(4)
3 0.138(5)

####################################################################### 
# 
# 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_wf446cs2
_database_code_depnum_ccdc_archive 'CCDC 2094043'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-07-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H36 N2 S3, C S2'
_chemical_formula_sum            'C31 H36 N2 S5'
_chemical_formula_weight         596.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H36 N2 S5'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.29535(12)
_cell_length_b                   10.67345(16)
_cell_length_c                   36.5755(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.0920(11)
_cell_angle_gamma                90
_cell_volume                     3236.24(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9656
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.3790
_cell_measurement_theta_min      4.2960
_shelx_estimated_absorpt_T_max   0.607
_shelx_estimated_absorpt_T_min   0.331
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1577
0 0 -1 0.1415
0 1 -2 0.1150
0 -1 2 0.1440
0 2 -1 0.0988
0 -2 1 0.1083
1 0 -2 0.1180
-1 0 2 0.1352
0 1 1 0.0790
0 -1 -1 0.0809
0 1 2 0.0843
1 -1 -1 0.1133
2 -1 -2 0.1070
2 1 1 0.1418
-1 -1 -2 0.1841
-2 1 -2 0.2036

_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
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
0.0000 0.0000 0.9999 -0.0359 0.0152 -0.0160
-0.0000 -0.0000 -0.9999 0.0359 -0.0152 0.0160
-0.0000 1.0000 -2.0000 0.1311 0.1009 0.0238
0.0000 -1.0000 2.0000 -0.1311 -0.1009 -0.0238
-0.0000 2.0000 -1.0002 0.1545 0.2475 -0.0005
0.0000 -2.0000 1.0002 -0.1545 -0.2475 0.0005
1.0000 -0.0000 -1.9999 0.0056 0.0100 0.2009
-1.0000 0.0000 1.9999 -0.0056 -0.0100 -0.2009
-0.0000 1.0000 0.9998 0.0234 0.1466 -0.0243
0.0000 -1.0000 -0.9998 -0.0234 -0.1466 0.0243
-0.0000 1.0000 1.9998 -0.0125 0.1618 -0.0403
1.0001 -1.0000 -0.9998 -0.0895 -0.1062 0.1932
2.0001 -1.0000 -1.9998 -0.1198 -0.0810 0.3781
2.0001 1.0000 0.9998 -0.1089 0.2273 0.3136
-1.0000 -1.0000 -1.9998 0.0786 -0.2022 -0.1286
-2.0001 1.0000 -2.0000 0.2634 0.0201 -0.3140

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            17191
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.679
_diffrn_reflns_theta_min         4.315
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -112.00 -65.00   1.00    1.00    --  -40.91-144.00-141.00   47
  2  ω    -88.00 -31.00   1.00    1.00    --  -40.91 126.00 103.00   57
  3  ω    -82.00 -57.00   1.00    1.00    --  -40.91 144.00 -87.00   25
  4  ω     56.00  81.00   1.00    1.00    --   40.91-126.00  27.00   25
  5  ω     49.00  74.00   1.00    1.00    --   40.91-144.00-141.00   25
  6  ω    100.00 130.00   1.00    1.17    --  105.15 144.00 -87.00   30
  7  ω     72.00 107.00   1.00    1.17    --  105.15-126.00  27.00   35
  8  ω    137.00 162.00   1.00    1.17    --  105.15 126.00 103.00   25
  9  ω     60.00  85.00   1.00    1.17    --  105.15-144.00-141.00   25
 10  ω   -101.00 -17.00   1.00    1.00    --  -40.91 -38.00 -90.00   84
 11  ω   -115.00 -17.00   1.00    1.00    --  -40.91 -38.00-180.00   98
 12  ω     49.00 133.00   1.00    1.17    --  105.15 -61.00-180.00   84
 13  ω     82.00 178.00   1.00    1.17    --  105.15  45.00 -90.00   96
 14  ω     30.00 109.00   1.00    1.17    --  105.15-111.00  60.00   79
 15  ω    104.00 174.00   1.00    1.17    --  105.15  77.00 120.00   70
 16  ω     44.00  97.00   1.00    1.17    --  105.15-111.00-150.00   53
 17  ω    134.00 159.00   1.00    1.17    --  105.15  77.00   0.00   25
 18  ω    106.00 131.00   1.00    1.17    --  105.15 111.00  60.00   25
 19  ω    103.00 129.00   1.00    1.17    --  105.15  77.00   0.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0661347000
_diffrn_orient_matrix_UB_12      0.0592878000
_diffrn_orient_matrix_UB_13      -0.0358931000
_diffrn_orient_matrix_UB_21      0.0403866000
_diffrn_orient_matrix_UB_22      0.1313440000
_diffrn_orient_matrix_UB_23      0.0152127000
_diffrn_orient_matrix_UB_31      0.1689090000
_diffrn_orient_matrix_UB_32      -0.0082465000
_diffrn_orient_matrix_UB_33      -0.0160171000
_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                5654
_reflns_number_total             6219
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00107(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6219
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0321
_refine_ls_restrained_S_all      1.082
_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)+(0.0378P)²+1.3198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0832
_refine_special_details          ?
_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. Restrained distances
 S5B-C33 \\sim S5A-C33 \\sim S4B-C33 \\sim S4A-C33
 with sigma of 0.005
 S4A-S5A \\sim S4B-S5B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S4A \\sim S4B \\sim S5A \\sim S5B \\sim C33: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(S4B)=Sof(S5B)=1-FVAR(1)
 Sof(S4A)=Sof(S5A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C27(H27), C30(H30)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C23(H23), C24(H24), C25(H25)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.37047(4) 0.70918(4) 0.58096(2) 0.02926(10) Uani 1 1 d . . . . .
S2 S 0.57007(5) 0.32614(4) 0.66905(2) 0.03782(11) Uani 1 1 d . . . . .
S3 S 0.29463(4) 0.46285(4) 0.62421(2) 0.02984(10) Uani 1 1 d . . . . .
N1 N 0.81293(13) 0.62208(11) 0.59775(3) 0.0195(2) Uani 1 1 d . . . . .
N2 N 0.81103(13) 0.62541(11) 0.65708(3) 0.0197(2) Uani 1 1 d . . . . .
C2 C 0.72145(16) 0.59560(12) 0.62673(3) 0.0189(3) Uani 1 1 d . . . . .
C4 C 0.95914(16) 0.67038(14) 0.64697(4) 0.0236(3) Uani 1 1 d . . . . .
H4 H 1.044389 0.698055 0.663043 0.028 Uiso 1 1 calc R U . . .
C5 C 0.96053(16) 0.66780(14) 0.61017(4) 0.0235(3) Uani 1 1 d . . . . .
H5 H 1.047045 0.692811 0.595492 0.028 Uiso 1 1 calc R U . . .
C6 C 0.56015(16) 0.54570(13) 0.62563(3) 0.0209(3) Uani 1 1 d . . . . .
C7 C 0.41928(16) 0.58975(14) 0.60699(4) 0.0232(3) Uani 1 1 d . . . . .
C8 C 0.49901(17) 0.43839(14) 0.64326(4) 0.0256(3) Uani 1 1 d . . . . .
C9 C 0.77041(16) 0.60007(13) 0.55942(3) 0.0201(3) Uani 1 1 d . . . . .
C10 C 0.75084(17) 0.70513(13) 0.53647(4) 0.0238(3) Uani 1 1 d . . . . .
C11 C 0.71748(19) 0.68115(15) 0.49961(4) 0.0303(3) Uani 1 1 d . . . . .
H11 H 0.704186 0.749462 0.483122 0.036 Uiso 1 1 calc R U . . .
C12 C 0.7032(2) 0.56040(16) 0.48642(4) 0.0337(4) Uani 1 1 d . . . . .
H12 H 0.679043 0.546665 0.461148 0.040 Uiso 1 1 calc R U . . .
C13 C 0.72390(19) 0.45965(15) 0.50965(4) 0.0304(3) Uani 1 1 d . . . . .
H13 H 0.713808 0.377092 0.500133 0.036 Uiso 1 1 calc R U . . .
C14 C 0.75938(17) 0.47665(14) 0.54692(4) 0.0234(3) Uani 1 1 d . . . . .
C15 C 0.7688(2) 0.83921(14) 0.54983(4) 0.0312(3) Uani 1 1 d . . . . .
H15 H 0.760411 0.839562 0.577031 0.037 Uiso 1 1 calc R U . . .
C16 C 0.9351(2) 0.89165(17) 0.54051(5) 0.0427(4) Uani 1 1 d . . . . .
H16A H 1.019835 0.837797 0.551310 0.064 Uiso 1 1 calc R U . . .
H16B H 0.946891 0.976614 0.550403 0.064 Uiso 1 1 calc R U . . .
H16C H 0.944440 0.893930 0.513888 0.064 Uiso 1 1 calc R U . . .
C17 C 0.6370(2) 0.92469(17) 0.53338(5) 0.0450(4) Uani 1 1 d . . . . .
H17A H 0.653088 0.935369 0.507154 0.068 Uiso 1 1 calc R U . . .
H17B H 0.642474 1.006552 0.545500 0.068 Uiso 1 1 calc R U . . .
H17C H 0.531074 0.886912 0.536961 0.068 Uiso 1 1 calc R U . . .
C18 C 0.78988(18) 0.36245(13) 0.57099(4) 0.0268(3) Uani 1 1 d . . . . .
H18 H 0.806787 0.391743 0.596814 0.032 Uiso 1 1 calc R U . . .
C19 C 0.9432(2) 0.29527(18) 0.55975(5) 0.0437(4) Uani 1 1 d . . . . .
H19A H 0.961740 0.221724 0.575383 0.065 Uiso 1 1 calc R U . . .
H19B H 1.035274 0.352429 0.562507 0.065 Uiso 1 1 calc R U . . .
H19C H 0.930752 0.268615 0.534165 0.065 Uiso 1 1 calc R U . . .
C20 C 0.6452(2) 0.27340(15) 0.56948(5) 0.0358(4) Uani 1 1 d . . . . .
H20A H 0.548029 0.319058 0.576102 0.054 Uiso 1 1 calc R U . . .
H20B H 0.664735 0.204286 0.586712 0.054 Uiso 1 1 calc R U . . .
H20C H 0.630232 0.239835 0.544645 0.054 Uiso 1 1 calc R U . . .
C21 C 0.75857(16) 0.62535(13) 0.69452(3) 0.0210(3) Uani 1 1 d . . . . .
C22 C 0.83355(17) 0.54215(13) 0.71951(4) 0.0242(3) Uani 1 1 d . . . . .
C23 C 0.78725(18) 0.55046(14) 0.75575(4) 0.0288(3) Uani 1 1 d . . . . .
H23 H 0.835232 0.495894 0.773551 0.035 Uiso 1 1 calc R U . . .
C24 C 0.67321(19) 0.63626(16) 0.76631(4) 0.0314(3) Uani 1 1 d . . . . .
H24 H 0.643755 0.639971 0.791148 0.038 Uiso 1 1 calc R U . . .
C25 C 0.60211(18) 0.71633(15) 0.74105(4) 0.0298(3) Uani 1 1 d . . . . .
H25 H 0.523658 0.774605 0.748718 0.036 Uiso 1 1 calc R U . . .
C26 C 0.64305(17) 0.71366(13) 0.70424(4) 0.0240(3) Uani 1 1 d . . . . .
C27 C 0.96356(19) 0.44953(15) 0.70954(4) 0.0317(3) Uani 1 1 d . . . . .
H27 H 0.960486 0.439889 0.682332 0.038 Uiso 1 1 calc R U . . .
C28 C 1.1311(2) 0.49890(19) 0.72173(5) 0.0422(4) Uani 1 1 d . . . . .
H28A H 1.149674 0.580208 0.710169 0.063 Uiso 1 1 calc R U . . .
H28B H 1.213846 0.439366 0.714393 0.063 Uiso 1 1 calc R U . . .
H28C H 1.136576 0.508601 0.748388 0.063 Uiso 1 1 calc R U . . .
C29 C 0.9379(2) 0.32007(17) 0.72663(5) 0.0460(4) Uani 1 1 d . . . . .
H29A H 0.957434 0.325128 0.753171 0.069 Uiso 1 1 calc R U . . .
H29B H 1.012969 0.259911 0.716297 0.069 Uiso 1 1 calc R U . . .
H29C H 0.826775 0.292501 0.721319 0.069 Uiso 1 1 calc R U . . .
C30 C 0.56654(17) 0.80792(14) 0.67782(4) 0.0270(3) Uani 1 1 d . . . . .
H30 H 0.599235 0.785652 0.652591 0.032 Uiso 1 1 calc R U . . .
C31 C 0.6286(2) 0.94030(16) 0.68646(5) 0.0408(4) Uani 1 1 d . . . . .
H31A H 0.596718 0.964656 0.710996 0.061 Uiso 1 1 calc R U . . .
H31B H 0.582313 0.999308 0.668433 0.061 Uiso 1 1 calc R U . . .
H31C H 0.746504 0.941575 0.685468 0.061 Uiso 1 1 calc R U . . .
C32 C 0.38203(19) 0.80181(17) 0.67848(5) 0.0369(4) Uani 1 1 d . . . . .
H32A H 0.346124 0.715935 0.673315 0.055 Uiso 1 1 calc R U . . .
H32B H 0.335229 0.858463 0.659868 0.055 Uiso 1 1 calc R U . . .
H32C H 0.346784 0.827131 0.702671 0.055 Uiso 1 1 calc R U . . .
S4A S 0.3214(4) 0.0856(5) 0.60140(12) 0.0959(12) Uani 0.580(8) 1 d D U P A 1
S4B S 0.3049(4) 0.0613(4) 0.59440(13) 0.0602(8) Uani 0.420(8) 1 d D U P A 2
S5A S 0.0114(2) 0.0454(4) 0.64299(6) 0.0847(9) Uani 0.580(8) 1 d D U P A 1
S5B S 0.0403(6) 0.1229(8) 0.64786(7) 0.1168(15) Uani 0.420(8) 1 d D U P A 2
C33 C 0.1675(2) 0.0744(2) 0.62191(5) 0.0676(6) Uani 1 1 d D 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
S1 C7 1.6332(15) . ?
S2 C8 1.6224(16) . ?
S3 C7 1.8297(15) . ?
S3 C8 1.8280(15) . ?
N1 C2 1.3558(16) . ?
N1 C5 1.3795(18) . ?
N1 C9 1.4523(16) . ?
N2 C2 1.3509(17) . ?
N2 C4 1.3819(17) . ?
N2 C21 1.4520(16) . ?
C2 C6 1.4394(19) . ?
C4 H4 0.9500 . ?
C4 C5 1.3468(19) . ?
C5 H5 0.9500 . ?
C6 C7 1.4117(19) . ?
C6 C8 1.417(2) . ?
C9 C10 1.4065(19) . ?
C9 C14 1.3963(19) . ?
C10 C11 1.390(2) . ?
C10 C15 1.518(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.380(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.396(2) . ?
C14 C18 1.519(2) . ?
C15 H15 1.0000 . ?
C15 C16 1.538(2) . ?
C15 C17 1.530(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.529(2) . ?
C18 C20 1.530(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.4035(19) . ?
C21 C26 1.3993(19) . ?
C22 C23 1.396(2) . ?
C22 C27 1.517(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.382(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.376(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.401(2) . ?
C26 C30 1.518(2) . ?
C27 H27 1.0000 . ?
C27 C28 1.537(2) . ?
C27 C29 1.534(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30 1.0000 . ?
C30 C31 1.533(2) . ?
C30 C32 1.533(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
S4A C33 1.509(3) . ?
S4B C33 1.554(3) . ?
S5A C33 1.562(2) . ?
S5B C33 1.535(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 S3 C7 73.08(7) . . ?
C2 N1 C5 109.38(11) . . ?
C2 N1 C9 126.72(11) . . ?
C5 N1 C9 123.81(11) . . ?
C2 N2 C4 109.26(11) . . ?
C2 N2 C21 126.86(11) . . ?
C4 N2 C21 123.53(11) . . ?
N1 C2 C6 126.97(12) . . ?
N2 C2 N1 106.64(11) . . ?
N2 C2 C6 126.38(11) . . ?
N2 C4 H4 126.3 . . ?
C5 C4 N2 107.48(12) . . ?
C5 C4 H4 126.3 . . ?
N1 C5 H5 126.4 . . ?
C4 C5 N1 107.24(12) . . ?
C4 C5 H5 126.4 . . ?
C7 C6 C2 129.99(13) . . ?
C7 C6 C8 100.67(12) . . ?
C8 C6 C2 129.34(13) . . ?
S1 C7 S3 130.33(8) . . ?
C6 C7 S1 136.44(11) . . ?
C6 C7 S3 93.18(10) . . ?
S2 C8 S3 129.75(9) . . ?
C6 C8 S2 137.13(12) . . ?
C6 C8 S3 93.06(10) . . ?
C10 C9 N1 117.76(12) . . ?
C14 C9 N1 118.65(12) . . ?
C14 C9 C10 123.50(12) . . ?
C9 C10 C15 123.49(12) . . ?
C11 C10 C9 116.52(13) . . ?
C11 C10 C15 119.97(13) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 C10 121.51(14) . . ?
C12 C11 H11 119.2 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.43(14) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.4 . . ?
C12 C13 C14 121.20(14) . . ?
C14 C13 H13 119.4 . . ?
C9 C14 C18 124.03(12) . . ?
C13 C14 C9 116.83(13) . . ?
C13 C14 C18 119.10(13) . . ?
C10 C15 H15 108.3 . . ?
C10 C15 C16 110.48(13) . . ?
C10 C15 C17 112.06(14) . . ?
C16 C15 H15 108.3 . . ?
C17 C15 H15 108.3 . . ?
C17 C15 C16 109.24(14) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18 108.1 . . ?
C14 C18 C19 110.05(12) . . ?
C14 C18 C20 111.32(13) . . ?
C19 C18 H18 108.1 . . ?
C19 C18 C20 110.97(14) . . ?
C20 C18 H18 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N2 118.27(12) . . ?
C26 C21 N2 118.10(12) . . ?
C26 C21 C22 123.50(12) . . ?
C21 C22 C27 123.90(12) . . ?
C23 C22 C21 116.58(13) . . ?
C23 C22 C27 119.48(13) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.49(14) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.33(13) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.33(14) . . ?
C26 C25 H25 119.3 . . ?
C21 C26 C25 116.77(13) . . ?
C21 C26 C30 123.98(12) . . ?
C25 C26 C30 119.21(13) . . ?
C22 C27 H27 108.3 . . ?
C22 C27 C28 110.49(14) . . ?
C22 C27 C29 112.23(14) . . ?
C28 C27 H27 108.3 . . ?
C29 C27 H27 108.3 . . ?
C29 C27 C28 109.16(14) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30 108.0 . . ?
C26 C30 C31 110.51(12) . . ?
C26 C30 C32 110.88(13) . . ?
C31 C30 H30 108.0 . . ?
C31 C30 C32 111.35(13) . . ?
C32 C30 H30 108.0 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
S4A C33 S5A 173.1(3) . . ?
S5B C33 S4B 165.4(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 C2 C6 C7 -54.4(2) . . . . ?
N1 C2 C6 C8 125.95(16) . . . . ?
N1 C9 C10 C11 177.13(12) . . . . ?
N1 C9 C10 C15 -1.2(2) . . . . ?
N1 C9 C14 C13 -177.78(12) . . . . ?
N1 C9 C14 C18 -0.2(2) . . . . ?
N2 C2 C6 C7 125.45(16) . . . . ?
N2 C2 C6 C8 -54.2(2) . . . . ?
N2 C4 C5 N1 0.40(16) . . . . ?
N2 C21 C22 C23 175.99(12) . . . . ?
N2 C21 C22 C27 -1.7(2) . . . . ?
N2 C21 C26 C25 -176.23(13) . . . . ?
N2 C21 C26 C30 1.3(2) . . . . ?
C2 N1 C5 C4 -0.51(16) . . . . ?
C2 N1 C9 C10 114.89(15) . . . . ?
C2 N1 C9 C14 -68.38(18) . . . . ?
C2 N2 C4 C5 -0.16(16) . . . . ?
C2 N2 C21 C22 116.95(15) . . . . ?
C2 N2 C21 C26 -66.94(18) . . . . ?
C2 C6 C7 S1 -2.1(2) . . . . ?
C2 C6 C7 S3 -179.77(13) . . . . ?
C2 C6 C8 S2 -3.2(3) . . . . ?
C2 C6 C8 S3 179.77(13) . . . . ?
C4 N2 C2 N1 -0.15(15) . . . . ?
C4 N2 C2 C6 179.98(13) . . . . ?
C4 N2 C21 C22 -70.52(18) . . . . ?
C4 N2 C21 C26 105.59(15) . . . . ?
C5 N1 C2 N2 0.40(15) . . . . ?
C5 N1 C2 C6 -179.73(13) . . . . ?
C5 N1 C9 C10 -69.04(17) . . . . ?
C5 N1 C9 C14 107.69(15) . . . . ?
C7 S3 C8 S2 -177.41(12) . . . . ?
C7 S3 C8 C6 -0.03(8) . . . . ?
C7 C6 C8 S2 177.07(14) . . . . ?
C7 C6 C8 S3 0.04(10) . . . . ?
C8 S3 C7 S1 -177.83(12) . . . . ?
C8 S3 C7 C6 0.03(8) . . . . ?
C8 C6 C7 S1 177.60(13) . . . . ?
C8 C6 C7 S3 -0.04(10) . . . . ?
C9 N1 C2 N2 176.94(12) . . . . ?
C9 N1 C2 C6 -3.2(2) . . . . ?
C9 N1 C5 C4 -177.17(12) . . . . ?
C9 C10 C11 C12 0.5(2) . . . . ?
C9 C10 C15 C16 100.64(16) . . . . ?
C9 C10 C15 C17 -137.30(15) . . . . ?
C9 C14 C18 C19 -112.13(16) . . . . ?
C9 C14 C18 C20 124.41(15) . . . . ?
C10 C9 C14 C13 -1.3(2) . . . . ?
C10 C9 C14 C18 176.28(13) . . . . ?
C10 C11 C12 C13 -0.8(2) . . . . ?
C11 C10 C15 C16 -77.60(18) . . . . ?
C11 C10 C15 C17 44.46(19) . . . . ?
C11 C12 C13 C14 0.1(2) . . . . ?
C12 C13 C14 C9 0.9(2) . . . . ?
C12 C13 C14 C18 -176.75(14) . . . . ?
C13 C14 C18 C19 65.35(18) . . . . ?
C13 C14 C18 C20 -58.11(17) . . . . ?
C14 C9 C10 C11 0.6(2) . . . . ?
C14 C9 C10 C15 -177.72(13) . . . . ?
C15 C10 C11 C12 178.83(15) . . . . ?
C21 N2 C2 N1 173.26(12) . . . . ?
C21 N2 C2 C6 -6.6(2) . . . . ?
C21 N2 C4 C5 -173.84(12) . . . . ?
C21 C22 C23 C24 0.1(2) . . . . ?
C21 C22 C27 C28 101.21(16) . . . . ?
C21 C22 C27 C29 -136.69(15) . . . . ?
C21 C26 C30 C31 -108.74(16) . . . . ?
C21 C26 C30 C32 127.30(15) . . . . ?
C22 C21 C26 C25 -0.3(2) . . . . ?
C22 C21 C26 C30 177.20(13) . . . . ?
C22 C23 C24 C25 0.0(2) . . . . ?
C23 C22 C27 C28 -76.37(17) . . . . ?
C23 C22 C27 C29 45.72(19) . . . . ?
C23 C24 C25 C26 -0.2(2) . . . . ?
C24 C25 C26 C21 0.4(2) . . . . ?
C24 C25 C26 C30 -177.28(14) . . . . ?
C25 C26 C30 C31 68.75(18) . . . . ?
C25 C26 C30 C32 -55.21(18) . . . . ?
C26 C21 C22 C23 0.1(2) . . . . ?
C26 C21 C22 C27 -177.54(14) . . . . ?
C27 C22 C23 C24 177.85(14) . . . . ?

_olex2_date_sample_data_collection 2021-04-22
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.273
_oxdiff_exptl_absorpt_empirical_full_min 0.724
####################################################################### 
# 
# 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_wf446hbr
_database_code_depnum_ccdc_archive 'CCDC 2094753'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-06-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.471(Br), 0.529(Cl), C H2 Cl2, C58 H73 N4 O2'
_chemical_formula_sum            'C59 H75 Br0.47 Cl2.53 N4 O2'
_chemical_formula_weight         999.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C61 H79 N4 O2 Cl6 Br1'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   24.5239(7)
_cell_length_b                   29.6444(9)
_cell_length_c                   16.5867(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.752(3)
_cell_angle_gamma                90
_cell_volume                     11997.8(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7195
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      68.2190
_cell_measurement_theta_min      3.5650
_shelx_estimated_absorpt_T_max   0.846
_shelx_estimated_absorpt_T_min   0.398
_exptl_absorpt_coefficient_mu    1.867
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4260
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -2 1 0.0476
1 2 -1 0.0459
1 -1 2 0.1558
-1 1 -2 0.1802
1 -1 -1 0.2736
2 -1 2 0.1723
-2 1 -2 0.1878
11 4 6 0.1627
-11 -5 -7 0.1944
7 -15 -6 0.2821
-12 -12 0 0.1374
11 14 1 0.1110
2 -19 -1 0.2265
6 15 -5 0.0395
11 11 -6 0.0970
-9 -13 6 0.0574
5 16 -5 0.0518
-13 6 -4 0.1573
0 9 10 0.2016
7 16 -4 0.0329
10 13 -5 0.0610
-5 -17 4 0.1070
-9 -14 5 0.0526
9 9 -8 0.1093

_exptl_crystal_size_max          0.605
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.093
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
-1.0001 -2.0002 1.0005 -0.0160 0.1486 -0.0039
1.0001 2.0002 -1.0005 0.0160 -0.1486 0.0039
0.9991 -0.9981 2.0014 -0.1661 0.1033 -0.0756
-0.9991 0.9981 -2.0014 0.1661 -0.1033 0.0756
1.0002 -1.0017 -1.0009 0.0776 -0.0351 -0.0836
1.9988 -0.9980 2.0014 -0.1902 0.0765 -0.1273
-1.9988 0.9980 -2.0014 0.1902 -0.0765 0.1273
11.3765 4.0222 6.3848 -0.8755 -0.1629 -0.4550
-10.8581 -4.8056 -6.6317 0.8991 0.1672 0.4046
6.5910 -14.6871 -5.7688 0.6098 0.1130 -0.7844
-12.3339 -11.9289 -0.4871 0.5823 0.7597 0.2894
10.6398 14.0806 0.6972 -0.6025 -0.7860 -0.1385
2.1244 -18.9241 -1.4493 0.4543 0.5923 -0.6654
6.4577 15.1134 -5.4284 -0.0256 -0.9954 0.0921
10.8814 10.8620 -5.6826 -0.0248 -0.9649 -0.2615
-8.5417 -13.4495 5.6285 0.0257 0.9976 0.0648
4.9999 16.0049 -5.0013 -0.0433 -0.9704 0.1947
-12.9960 5.9977 -4.0022 0.5159 -0.0630 0.8371
-0.0044 9.0179 10.0092 -0.9968 0.1204 0.2893
6.9991 16.0063 -4.0005 -0.1729 -0.9779 0.0939
9.9990 13.0035 -5.0018 -0.1026 -0.9909 -0.1516
-4.9995 -17.0067 4.0004 0.1451 0.9621 -0.2265
-8.9992 -14.0040 5.0016 0.0989 1.0019 0.0707
9.0007 8.9972 -8.0047 0.2473 -0.9510 -0.2246

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.610
_diffrn_reflns_theta_min         2.981
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00   9.00   1.00   10.00    --  -43.13  75.00 125.00   83
  2  ω     25.00  51.00   1.00   10.00    --   43.13 -75.00  -2.00   26
  3  ω    105.00 166.00   1.00   40.00    --  103.80  75.00 125.00   61
  4  ω     35.00 132.00   1.00   40.00    --  103.80 -75.00  -2.00   97
  5  ω     -7.00  30.00   1.00   10.00    --  -43.13  37.00   0.00   37
  6  ω   -117.00 -19.00   1.00   10.00    --  -43.13 -37.00-180.00   98
  7  ω     41.00  69.00   1.00   10.00    --   43.13 -99.00-180.00   28
  8  ω     47.00 108.00   1.00   40.00    --  103.80-111.00-150.00   61
  9  ω     29.00 129.00   1.00   40.00    --  103.80 -30.00   0.00  100
 10  ω    126.00 153.00   1.00   40.00    --  103.80 111.00   0.00   27
 11  ω    106.00 177.00   1.00   40.00    --  103.80 111.00  90.00   71
 12  ω     28.00  96.00   1.00   40.00    --  103.80-111.00 -60.00   68
 13  ω    107.00 163.00   1.00   40.00    --  103.80 111.00 -30.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0241752000
_diffrn_orient_matrix_UB_12      -0.0205058000
_diffrn_orient_matrix_UB_13      -0.0811278000
_diffrn_orient_matrix_UB_21      -0.0268170000
_diffrn_orient_matrix_UB_22      -0.0378414000
_diffrn_orient_matrix_UB_23      0.0461146000
_diffrn_orient_matrix_UB_31      -0.0517649000
_diffrn_orient_matrix_UB_32      0.0291521000
_diffrn_orient_matrix_UB_33      0.0026140000
_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                12412
_reflns_number_total             23200
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1356
_refine_ls_number_reflns         23200
_refine_ls_number_restraints     1203
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0727
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0987P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.2142
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C121-C118 \\sim C117-C122
 with sigma of 0.02
 C121-C116 \\sim C117-C116 \\sim C118-C116 \\sim C122-C116
 with sigma of 0.02
 C80-C123 \\sim C82-C80 \\sim C81-C80 \\sim C80-C124
 with sigma of 0.02
 C123-C124 \\sim C82-C81
 with sigma of 0.02
 Cl7-C119 \\sim Cl4-C119 \\sim Cl3-C119 \\sim Cl8-C119
 with sigma of 0.02
 Cl7-Cl8 \\sim Cl4-Cl3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Br1 \\sim Cl2 \\sim Cl1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C119 \\sim Cl7 \\sim Cl4 \\sim Cl8 \\sim Cl3: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(Cl1) = Uanis(Br1) = Uanis(Br2) = Uanis(Cl2)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl2)=Sof(Cl1)=1-FVAR(1)
 Sof(Br1)=Sof(Br2)=FVAR(1)
 Sof(O5)=Sof(O6)=Sof(H62A)=Sof(C65)=Sof(C66)=1-FVAR(2)
 Sof(O3)=Sof(O4)=Sof(H62)=Sof(C63)=Sof(C64)=FVAR(2)
 Sof(H11G)=Sof(C117)=Sof(H11H)=Sof(H11I)=Sof(H11J)=Sof(C122)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=1-FVAR(3)
 Sof(H116)=Sof(C118)=Sof(H11K)=Sof(H11L)=Sof(H11M)=Sof(C121)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=FVAR(3)
 Sof(H80A)=Sof(C124)=Sof(H12G)=Sof(H12H)=Sof(H12I)=Sof(C123)=Sof(H12J)=
 Sof(H12K)=Sof(H12L)=1-FVAR(4)
 Sof(H80)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=
 Sof(H82C)=FVAR(4)
 Sof(H11P)=Sof(H11Q)=Sof(Cl7)=Sof(Cl8)=1-FVAR(5)
 Sof(Cl3)=Sof(Cl4)=Sof(H11N)=Sof(H11O)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C17(H17), C20(H20), C29(H29), C32(H32), C41(H41), C44(H44), C53(H53),
 C56(H56), C62(H62), C62(H62A), C77(H77), C80(H80), C80(H80A), C89(H89),
 C92(H92), C101(H101), C104(H104), C113(H113), C116(H11G), C116(H116)
6.b Secondary CH2 refined with riding coordinates:
 C119(H11N,H11O), C119(H11P,H11Q), C120(H12M,H12N)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C25(H25),
 C26(H26), C27(H27), C37(H37), C38(H38), C39(H39), C49(H49), C50(H50), C51(H51),
  C60(H60), C61(H61), C69(H69), C70(H70), C73(H73), C74(H74), C75(H75),
 C85(H85), C86(H86), C87(H87), C97(H97), C98(H98), C99(H99), C109(H109),
 C110(H110), C111(H111)
6.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,
 H81B,H81C), C82(H82A,H82B,H82C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C),
 C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C102(H10A,H10B,H10C), C103(H10D,H10E,
 H10F), C105(H10G,H10H,H10I), C106(H10J,H10K,H10L), C114(H11A,H11B,H11C),
 C115(H11D,H11E,H11F), C117(H11H,H11I,H11J), C118(H11K,H11L,H11M), C122(H12A,
 H12B,H12C), C121(H12D,H12E,H12F), C124(H12G,H12H,H12I), C123(H12J,H12K,H12L)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.00536(8) 0.36294(8) 0.86009(17) 0.0428(3) Uani 0.471(3) 1 d . U P A 1
Br2 Br 0.44683(8) 0.34990(9) 0.25626(17) 0.0428(3) Uani 0.471(3) 1 d . . P A 1
Cl2 Cl 0.44400(18) 0.3547(2) 0.2400(4) 0.0428(3) Uani 0.529(3) 1 d . . P A 2
Cl1 Cl -0.00883(17) 0.35621(17) 0.8443(4) 0.0428(3) Uani 0.529(3) 1 d . U P A 2
Cl3 Cl 0.4971(7) 0.5640(8) 0.5213(8) 0.100(4) Uani 0.30(3) 1 d D U P B 1
Cl4 Cl 0.4270(5) 0.5603(10) 0.6477(12) 0.110(4) Uani 0.30(3) 1 d D U P B 1
C119 C 0.4958(2) 0.5561(2) 0.6278(4) 0.0758(16) Uani 1 1 d D U . . .
H11N H 0.510627 0.526012 0.644181 0.091 Uiso 0.30(3) 1 calc R U P B 1
H11O H 0.518145 0.579402 0.658234 0.091 Uiso 0.30(3) 1 calc R U P B 1
H11P H 0.517319 0.527768 0.630067 0.091 Uiso 0.70(3) 1 calc R U P B 2
H11Q H 0.516880 0.578789 0.661664 0.091 Uiso 0.70(3) 1 calc R U P B 2
Cl5 Cl 0.06036(8) 0.56044(6) 0.37979(11) 0.0896(5) Uani 1 1 d . . . . .
Cl6 Cl 0.14944(5) 0.58808(4) 0.28677(8) 0.0600(3) Uani 1 1 d . . . . .
C120 C 0.0837(2) 0.5640(2) 0.2831(3) 0.0649(14) Uani 1 1 d . . . . .
H12M H 0.084525 0.533435 0.259334 0.078 Uiso 1 1 calc R U . . .
H12N H 0.057699 0.582522 0.247464 0.078 Uiso 1 1 calc R U . . .
O1 O 0.30705(11) 0.73955(10) 1.0128(2) 0.0465(7) Uani 1 1 d . . . . .
O2 O 0.25025(11) 0.60825(11) 0.8976(2) 0.0488(8) Uani 1 1 d . . . . .
N1 N 0.41804(11) 0.68659(11) 0.93184(18) 0.0292(6) Uani 1 1 d . . . . .
N2 N 0.38251(11) 0.63576(11) 0.84860(18) 0.0312(6) Uani 1 1 d . . . . .
N3 N 0.18999(12) 0.65923(11) 1.07834(19) 0.0321(6) Uani 1 1 d . . . . .
N4 N 0.14255(11) 0.70215(11) 0.99249(18) 0.0318(6) Uani 1 1 d . . . . .
C1 C 0.37171(13) 0.66247(12) 0.9112(2) 0.0261(6) Uani 1 1 d . . . . .
C2 C 0.45701(15) 0.67480(14) 0.8798(2) 0.0343(8) Uani 1 1 d . . . . .
H2 H 0.492942 0.686877 0.880563 0.041 Uiso 1 1 calc R U . . .
C3 C 0.43496(14) 0.64376(14) 0.8290(2) 0.0350(8) Uani 1 1 d . . . . .
H3 H 0.452167 0.629611 0.786863 0.042 Uiso 1 1 calc R U . . .
C4 C 0.31939(14) 0.66768(13) 0.9416(2) 0.0317(7) Uani 1 1 d . . . . .
C5 C 0.29321(14) 0.70461(13) 0.9771(2) 0.0312(7) Uani 1 1 d . . . . .
C6 C 0.26766(15) 0.64376(14) 0.9244(2) 0.0343(7) Uani 1 1 d . . . . .
C7 C 0.23528(14) 0.68471(14) 0.9535(2) 0.0340(7) Uani 1 1 d . . . . .
H7 H 0.219498 0.701100 0.903809 0.041 Uiso 1 1 calc R U . . .
C8 C 0.19138(14) 0.68131(13) 1.0080(2) 0.0290(7) Uani 1 1 d . . . . .
C9 C 0.13981(15) 0.66689(14) 1.1077(2) 0.0351(8) Uani 1 1 d . . . . .
H9 H 0.128367 0.655348 1.156741 0.042 Uiso 1 1 calc R U . . .
C10 C 0.11048(15) 0.69342(15) 1.0547(2) 0.0368(8) Uani 1 1 d . . . . .
H10 H 0.074419 0.704246 1.058927 0.044 Uiso 1 1 calc R U . . .
C11 C 0.43315(13) 0.71219(13) 1.0052(2) 0.0287(6) Uani 1 1 d . . . . .
C12 C 0.43447(13) 0.75954(13) 1.0013(2) 0.0293(6) Uani 1 1 d . . . . .
C13 C 0.45484(14) 0.78235(14) 1.0714(2) 0.0338(7) Uani 1 1 d . . . . .
H13 H 0.456891 0.814348 1.070925 0.041 Uiso 1 1 calc R U . . .
C14 C 0.47205(15) 0.75922(15) 1.1414(2) 0.0361(8) Uani 1 1 d . . . . .
H14 H 0.485643 0.775401 1.188616 0.043 Uiso 1 1 calc R U . . .
C15 C 0.46971(15) 0.71298(15) 1.1434(2) 0.0365(8) Uani 1 1 d . . . . .
H15 H 0.481107 0.697778 1.192645 0.044 Uiso 1 1 calc R U . . .
C16 C 0.45101(14) 0.68755(14) 1.0750(2) 0.0337(7) Uani 1 1 d . . . . .
C17 C 0.41728(15) 0.78499(14) 0.9234(2) 0.0346(7) Uani 1 1 d . . . . .
H17 H 0.396477 0.763764 0.884867 0.042 Uiso 1 1 calc R U . . .
C18 C 0.38010(17) 0.82515(15) 0.9372(3) 0.0400(9) Uani 1 1 d . . . . .
H18A H 0.400411 0.847199 0.972515 0.060 Uiso 1 1 calc R U . . .
H18B H 0.348085 0.814671 0.962796 0.060 Uiso 1 1 calc R U . . .
H18C H 0.368003 0.839286 0.885032 0.060 Uiso 1 1 calc R U . . .
C19 C 0.46817(18) 0.80095(18) 0.8848(3) 0.0541(12) Uani 1 1 d . . . . .
H19A H 0.456799 0.817227 0.834525 0.081 Uiso 1 1 calc R U . . .
H19B H 0.490397 0.774778 0.872824 0.081 Uiso 1 1 calc R U . . .
H19C H 0.489837 0.821030 0.922490 0.081 Uiso 1 1 calc R U . . .
C20 C 0.45267(17) 0.63669(15) 1.0766(3) 0.0426(8) Uani 1 1 d . . . . .
H20 H 0.426186 0.625606 1.031133 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4353(3) 0.6169(2) 1.1551(4) 0.0719(16) Uani 1 1 d . . . . .
H21A H 0.461178 0.626442 1.200769 0.108 Uiso 1 1 calc R U . . .
H21B H 0.435043 0.583901 1.151619 0.108 Uiso 1 1 calc R U . . .
H21C H 0.398461 0.627670 1.163336 0.108 Uiso 1 1 calc R U . . .
C22 C 0.50944(19) 0.61894(17) 1.0621(3) 0.0567(12) Uani 1 1 d . . . . .
H22A H 0.518705 0.629038 1.008883 0.085 Uiso 1 1 calc R U . . .
H22B H 0.509305 0.585900 1.063823 0.085 Uiso 1 1 calc R U . . .
H22C H 0.536682 0.630524 1.104296 0.085 Uiso 1 1 calc R U . . .
C23 C 0.34813(15) 0.60049(14) 0.8097(2) 0.0341(7) Uani 1 1 d . . . . .
C24 C 0.31274(15) 0.61202(15) 0.7418(2) 0.0374(7) Uani 1 1 d . . . . .
C25 C 0.28357(17) 0.57642(16) 0.7023(3) 0.0436(9) Uani 1 1 d . . . . .
H25 H 0.258468 0.582835 0.656351 0.052 Uiso 1 1 calc R U . . .
C26 C 0.29007(19) 0.53255(17) 0.7279(3) 0.0497(10) Uani 1 1 d . . . . .
H26 H 0.270419 0.508959 0.699193 0.060 Uiso 1 1 calc R U . . .
C27 C 0.32541(18) 0.52304(16) 0.7958(3) 0.0461(9) Uani 1 1 d . . . . .
H27 H 0.328933 0.492805 0.814623 0.055 Uiso 1 1 calc R U . . .
C28 C 0.35594(16) 0.55673(15) 0.8373(3) 0.0396(7) Uani 1 1 d . . . . .
C29 C 0.30705(16) 0.65912(16) 0.7099(3) 0.0423(8) Uani 1 1 d . . . . .
H29 H 0.329487 0.679158 0.748774 0.051 Uiso 1 1 calc R U . . .
C30 C 0.24803(18) 0.67590(18) 0.7047(3) 0.0511(11) Uani 1 1 d . . . . .
H30A H 0.224748 0.656350 0.668099 0.077 Uiso 1 1 calc R U . . .
H30B H 0.246285 0.706855 0.683836 0.077 Uiso 1 1 calc R U . . .
H30C H 0.235129 0.675277 0.758696 0.077 Uiso 1 1 calc R U . . .
C31 C 0.33026(19) 0.66280(18) 0.6279(3) 0.0530(11) Uani 1 1 d . . . . .
H31A H 0.368792 0.653469 0.633688 0.080 Uiso 1 1 calc R U . . .
H31B H 0.327520 0.694104 0.608904 0.080 Uiso 1 1 calc R U . . .
H31C H 0.309338 0.643188 0.588521 0.080 Uiso 1 1 calc R U . . .
C32 C 0.39430(19) 0.54491(16) 0.9130(3) 0.0508(10) Uani 1 1 d . . . . .
H32 H 0.419998 0.570882 0.923970 0.061 Uiso 1 1 calc R U . . .
C33 C 0.3609(2) 0.5403(2) 0.9868(3) 0.0682(14) Uani 1 1 d . . . . .
H33A H 0.340588 0.568223 0.993671 0.102 Uiso 1 1 calc R U . . .
H33B H 0.385936 0.534566 1.035607 0.102 Uiso 1 1 calc R U . . .
H33C H 0.335170 0.515079 0.977898 0.102 Uiso 1 1 calc R U . . .
C34 C 0.4291(3) 0.5031(3) 0.9016(5) 0.104(2) Uani 1 1 d . . . . .
H34A H 0.405075 0.477551 0.885623 0.156 Uiso 1 1 calc R U . . .
H34B H 0.451181 0.496102 0.952534 0.156 Uiso 1 1 calc R U . . .
H34C H 0.453318 0.508925 0.859183 0.156 Uiso 1 1 calc R U . . .
C35 C 0.22928(15) 0.62768(14) 1.1165(2) 0.0339(7) Uani 1 1 d . . . . .
C36 C 0.26721(15) 0.64346(15) 1.1789(2) 0.0375(7) Uani 1 1 d . . . . .
C37 C 0.29991(17) 0.61114(15) 1.2203(3) 0.0445(9) Uani 1 1 d . . . . .
H37 H 0.325825 0.620315 1.263564 0.053 Uiso 1 1 calc R U . . .
C38 C 0.29589(18) 0.56691(16) 1.2006(3) 0.0482(10) Uani 1 1 d . . . . .
H38 H 0.319281 0.545661 1.229650 0.058 Uiso 1 1 calc R U . . .
C39 C 0.25813(17) 0.55230(15) 1.1388(3) 0.0439(9) Uani 1 1 d . . . . .
H39 H 0.256170 0.521157 1.125248 0.053 Uiso 1 1 calc R U . . .
C40 C 0.22319(16) 0.58242(15) 1.0963(3) 0.0395(7) Uani 1 1 d . . . . .
C41 C 0.27116(16) 0.69321(15) 1.2028(3) 0.0404(8) Uani 1 1 d . . . . .
H41 H 0.249273 0.711056 1.159796 0.048 Uiso 1 1 calc R U . . .
C42 C 0.2461(2) 0.70042(18) 1.2827(3) 0.0532(11) Uani 1 1 d . . . . .
H42A H 0.206862 0.693345 1.275133 0.080 Uiso 1 1 calc R U . . .
H42B H 0.251056 0.731933 1.299735 0.080 Uiso 1 1 calc R U . . .
H42C H 0.264255 0.680603 1.324402 0.080 Uiso 1 1 calc R U . . .
C43 C 0.33039(17) 0.71012(16) 1.2086(3) 0.0465(10) Uani 1 1 d . . . . .
H43A H 0.352885 0.692430 1.249316 0.070 Uiso 1 1 calc R U . . .
H43B H 0.331497 0.741989 1.224383 0.070 Uiso 1 1 calc R U . . .
H43C H 0.344718 0.706763 1.155865 0.070 Uiso 1 1 calc R U . . .
C44 C 0.17773(18) 0.56574(16) 1.0328(3) 0.0474(9) Uani 1 1 d . . . . .
H44 H 0.167307 0.591327 0.995087 0.057 Uiso 1 1 calc R U . . .
C45 C 0.12673(18) 0.5518(2) 1.0727(3) 0.0583(13) Uani 1 1 d . . . . .
H45A H 0.135976 0.526847 1.110446 0.088 Uiso 1 1 calc R U . . .
H45B H 0.098049 0.542049 1.030949 0.088 Uiso 1 1 calc R U . . .
H45C H 0.113480 0.577487 1.102389 0.088 Uiso 1 1 calc R U . . .
C46 C 0.1960(2) 0.52629(18) 0.9823(3) 0.0637(13) Uani 1 1 d . . . . .
H46A H 0.229885 0.534416 0.959060 0.095 Uiso 1 1 calc R U . . .
H46B H 0.167306 0.519542 0.938494 0.095 Uiso 1 1 calc R U . . .
H46C H 0.202542 0.499669 1.016932 0.095 Uiso 1 1 calc R U . . .
C47 C 0.12362(14) 0.72667(15) 0.9195(2) 0.0334(7) Uani 1 1 d . . . . .
C48 C 0.12120(14) 0.77311(15) 0.9221(2) 0.0356(7) Uani 1 1 d . . . . .
C49 C 0.09894(15) 0.79577(16) 0.8531(2) 0.0409(8) Uani 1 1 d . . . . .
H49 H 0.096008 0.827716 0.853804 0.049 Uiso 1 1 calc R U . . .
C50 C 0.08100(16) 0.77225(17) 0.7833(3) 0.0454(9) Uani 1 1 d . . . . .
H50 H 0.065537 0.788000 0.736627 0.054 Uiso 1 1 calc R U . . .
C51 C 0.08563(16) 0.72589(17) 0.7817(3) 0.0445(8) Uani 1 1 d . . . . .
H51 H 0.074342 0.710393 0.732724 0.053 Uiso 1 1 calc R U . . .
C52 C 0.10641(15) 0.70067(16) 0.8498(2) 0.0393(7) Uani 1 1 d . . . . .
C53 C 0.14210(16) 0.80010(15) 0.9975(2) 0.0394(8) Uani 1 1 d . . . . .
H53 H 0.157152 0.778302 1.040066 0.047 Uiso 1 1 calc R U . . .
C54 C 0.1885(2) 0.83144(19) 0.9785(3) 0.0585(13) Uani 1 1 d . . . . .
H54A H 0.219119 0.813466 0.962227 0.088 Uiso 1 1 calc R U . . .
H54B H 0.200898 0.849147 1.026785 0.088 Uiso 1 1 calc R U . . .
H54C H 0.175352 0.851834 0.934267 0.088 Uiso 1 1 calc R U . . .
C55 C 0.0956(2) 0.8262(2) 1.0308(3) 0.0663(15) Uani 1 1 d . . . . .
H55A H 0.081101 0.848678 0.990850 0.100 Uiso 1 1 calc R U . . .
H55B H 0.109508 0.841529 1.081078 0.100 Uiso 1 1 calc R U . . .
H55C H 0.066328 0.805295 1.041812 0.100 Uiso 1 1 calc R U . . .
C56 C 0.10931(16) 0.64984(17) 0.8493(3) 0.0462(8) Uani 1 1 d . . . . .
H56 H 0.143560 0.640626 0.883140 0.055 Uiso 1 1 calc R U . . .
C57 C 0.06061(19) 0.62878(17) 0.8866(3) 0.0535(11) Uani 1 1 d . . . . .
H57A H 0.061314 0.638104 0.943384 0.080 Uiso 1 1 calc R U . . .
H57B H 0.062995 0.595830 0.883679 0.080 Uiso 1 1 calc R U . . .
H57C H 0.026347 0.638929 0.856589 0.080 Uiso 1 1 calc R U . . .
C58 C 0.1117(2) 0.6306(2) 0.7640(3) 0.0623(13) Uani 1 1 d . . . . .
H58A H 0.076242 0.634895 0.732239 0.093 Uiso 1 1 calc R U . . .
H58B H 0.120186 0.598262 0.767792 0.093 Uiso 1 1 calc R U . . .
H58C H 0.140321 0.646159 0.737553 0.093 Uiso 1 1 calc R U . . .
O3 O 0.23415(17) 0.43464(15) 0.5963(3) 0.0568(14) Uani 0.767(6) 1 d . . P C 1
O4 O 0.19971(15) 0.30013(14) 0.4772(3) 0.0546(13) Uani 0.767(6) 1 d . . P C 1
O5 O 0.2042(6) 0.4377(5) 0.5220(11) 0.063(5) Uani 0.233(6) 1 d . . P C 2
O6 O 0.2323(5) 0.2889(5) 0.5658(10) 0.051(4) Uani 0.233(6) 1 d . . P C 2
N5 N 0.35530(12) 0.34299(12) 0.5027(2) 0.0337(6) Uani 1 1 d . . . . .
N6 N 0.30981(13) 0.38565(13) 0.4146(2) 0.0397(7) Uani 1 1 d . . . . .
N7 N 0.12064(13) 0.37677(13) 0.6694(2) 0.0445(8) Uani 1 1 d . . . . .
N8 N 0.08094(12) 0.34261(12) 0.5644(2) 0.0391(7) Uani 1 1 d . . . . .
C59 C 0.30741(14) 0.36490(14) 0.4861(2) 0.0321(7) Uani 1 1 d . . . . .
C60 C 0.38764(15) 0.34976(15) 0.4403(3) 0.0387(8) Uani 1 1 d . . . . .
H60 H 0.423309 0.337899 0.436749 0.046 Uiso 1 1 calc R U . . .
C61 C 0.35917(16) 0.37623(16) 0.3857(3) 0.0435(10) Uani 1 1 d . . . . .
H61 H 0.370956 0.386597 0.336147 0.052 Uiso 1 1 calc R U . . .
C62 C 0.26203(15) 0.36080(15) 0.5371(3) 0.0388(8) Uani 1 1 d . . . . .
H62 H 0.279089 0.345056 0.586635 0.047 Uiso 0.767(6) 1 calc R U P C 1
H62A H 0.280758 0.365968 0.592663 0.047 Uiso 0.233(6) 1 calc R U P C 2
C63 C 0.2251(2) 0.3970(2) 0.5714(4) 0.0384(13) Uani 0.767(6) 1 d . . P C 1
C64 C 0.2085(2) 0.33459(19) 0.5154(4) 0.0347(11) Uani 0.767(6) 1 d . . P C 1
C65 C 0.2268(7) 0.3291(7) 0.5496(12) 0.034(3) Uani 0.233(6) 1 d . . P C 2
C66 C 0.2142(8) 0.3976(8) 0.5317(15) 0.044(5) Uani 0.233(6) 1 d . . P C 2
C67 C 0.17778(15) 0.36619(15) 0.5555(3) 0.0416(8) Uani 1 1 d . . . . .
C68 C 0.12811(14) 0.36283(14) 0.5941(3) 0.0358(8) Uani 1 1 d . . . . .
C69 C 0.06868(17) 0.36487(16) 0.6882(3) 0.0491(11) Uani 1 1 d . . . . .
H69 H 0.053350 0.370644 0.737571 0.059 Uiso 1 1 calc R U . . .
C70 C 0.04433(16) 0.34354(15) 0.6226(3) 0.0452(10) Uani 1 1 d . . . . .
H70 H 0.008357 0.331283 0.617291 0.054 Uiso 1 1 calc R U . . .
C71 C 0.37160(14) 0.31839(14) 0.5767(2) 0.0342(7) Uani 1 1 d . . . . .
C72 C 0.36900(14) 0.27142(14) 0.5751(2) 0.0354(7) Uani 1 1 d . . . . .
C73 C 0.38535(16) 0.24909(16) 0.6470(3) 0.0416(8) Uani 1 1 d . . . . .
H73 H 0.384408 0.217059 0.648331 0.050 Uiso 1 1 calc R U . . .
C74 C 0.40302(16) 0.27262(17) 0.7170(3) 0.0443(8) Uani 1 1 d . . . . .
H74 H 0.413707 0.256607 0.765637 0.053 Uiso 1 1 calc R U . . .
C75 C 0.40522(17) 0.31911(17) 0.7165(3) 0.0461(9) Uani 1 1 d . . . . .
H75 H 0.417358 0.334708 0.765081 0.055 Uiso 1 1 calc R U . . .
C76 C 0.38990(16) 0.34373(15) 0.6459(3) 0.0410(8) Uani 1 1 d . . . . .
C77 C 0.34950(17) 0.24475(15) 0.4997(3) 0.0423(8) Uani 1 1 d . . . . .
H77 H 0.334219 0.266546 0.457309 0.051 Uiso 1 1 calc R U . . .
C78 C 0.3043(2) 0.2117(2) 0.5153(3) 0.0635(13) Uani 1 1 d . . . . .
H78A H 0.318851 0.189041 0.554854 0.095 Uiso 1 1 calc R U . . .
H78B H 0.290995 0.196643 0.464441 0.095 Uiso 1 1 calc R U . . .
H78C H 0.274093 0.227952 0.536499 0.095 Uiso 1 1 calc R U . . .
C79 C 0.3972(2) 0.2202(2) 0.4673(4) 0.0657(14) Uani 1 1 d . . . . .
H79A H 0.425237 0.242114 0.455532 0.099 Uiso 1 1 calc R U . . .
H79B H 0.384128 0.204004 0.417622 0.099 Uiso 1 1 calc R U . . .
H79C H 0.412967 0.198651 0.508020 0.099 Uiso 1 1 calc R U . . .
C80 C 0.39355(19) 0.39467(17) 0.6457(3) 0.0573(10) Uani 1 1 d D . . . .
H80 H 0.382556 0.404937 0.588989 0.069 Uiso 0.776(17) 1 calc R U P D 1
H80A H 0.362824 0.404386 0.605248 0.069 Uiso 0.224(17) 1 calc R U P D 2
C81 C 0.4526(3) 0.4113(3) 0.6689(7) 0.074(3) Uani 0.776(17) 1 d D . P D 1
H81A H 0.463155 0.405091 0.726397 0.111 Uiso 0.776(17) 1 calc R U P D 1
H81B H 0.454443 0.443886 0.659249 0.111 Uiso 0.776(17) 1 calc R U P D 1
H81C H 0.477593 0.395642 0.635949 0.111 Uiso 0.776(17) 1 calc R U P D 1
C82 C 0.3558(5) 0.4171(5) 0.6990(10) 0.108(5) Uani 0.776(17) 1 d D . P D 1
H82A H 0.318395 0.405871 0.685447 0.161 Uiso 0.776(17) 1 calc R U P D 1
H82B H 0.356496 0.449810 0.690497 0.161 Uiso 0.776(17) 1 calc R U P D 1
H82C H 0.367722 0.410322 0.755843 0.161 Uiso 0.776(17) 1 calc R U P D 1
C83 C 0.26916(16) 0.41463(16) 0.3710(3) 0.0424(8) Uani 1 1 d . . . . .
C84 C 0.23632(16) 0.39566(16) 0.3064(3) 0.0440(8) Uani 1 1 d . . . . .
C85 C 0.20278(18) 0.42506(17) 0.2593(3) 0.0516(10) Uani 1 1 d . . . . .
H85 H 0.179783 0.413612 0.214466 0.062 Uiso 1 1 calc R U . . .
C86 C 0.2020(2) 0.47030(18) 0.2760(3) 0.0572(11) Uani 1 1 d . . . . .
H86 H 0.178671 0.489602 0.242358 0.069 Uiso 1 1 calc R U . . .
C87 C 0.23470(19) 0.48846(18) 0.3410(3) 0.0557(11) Uani 1 1 d . . . . .
H87 H 0.233168 0.519795 0.352569 0.067 Uiso 1 1 calc R U . . .
C88 C 0.26989(18) 0.46021(17) 0.3895(3) 0.0477(9) Uani 1 1 d . . . . .
C89 C 0.23701(19) 0.34580(17) 0.2858(3) 0.0507(9) Uani 1 1 d . . . . .
H89 H 0.258098 0.329663 0.331855 0.061 Uiso 1 1 calc R U . . .
C90 C 0.1787(2) 0.3258(2) 0.2745(4) 0.0661(14) Uani 1 1 d . . . . .
H90A H 0.161430 0.328919 0.324956 0.099 Uiso 1 1 calc R U . . .
H90B H 0.180737 0.293733 0.260380 0.099 Uiso 1 1 calc R U . . .
H90C H 0.156871 0.341868 0.230855 0.099 Uiso 1 1 calc R U . . .
C91 C 0.2661(2) 0.3379(2) 0.2093(3) 0.0660(14) Uani 1 1 d . . . . .
H91A H 0.246840 0.354406 0.163761 0.099 Uiso 1 1 calc R U . . .
H91B H 0.266052 0.305621 0.196740 0.099 Uiso 1 1 calc R U . . .
H91C H 0.303982 0.348729 0.218485 0.099 Uiso 1 1 calc R U . . .
C92 C 0.3093(2) 0.48123(19) 0.4567(3) 0.0585(11) Uani 1 1 d . . . . .
H92 H 0.318715 0.457292 0.498238 0.070 Uiso 1 1 calc R U . . .
C93 C 0.3624(2) 0.4948(2) 0.4219(4) 0.0753(16) Uani 1 1 d . . . . .
H93A H 0.376167 0.469191 0.392544 0.113 Uiso 1 1 calc R U . . .
H93B H 0.389790 0.503589 0.466172 0.113 Uiso 1 1 calc R U . . .
H93C H 0.355171 0.520267 0.384709 0.113 Uiso 1 1 calc R U . . .
C94 C 0.2859(2) 0.5209(2) 0.4997(4) 0.0720(15) Uani 1 1 d . . . . .
H94A H 0.282149 0.546846 0.462974 0.108 Uiso 1 1 calc R U . . .
H94B H 0.310692 0.528672 0.547769 0.108 Uiso 1 1 calc R U . . .
H94C H 0.249931 0.512779 0.516129 0.108 Uiso 1 1 calc R U . . .
C95 C 0.16039(17) 0.39890(16) 0.7271(3) 0.0436(8) Uani 1 1 d . . . . .
C96 C 0.19905(18) 0.37178(17) 0.7717(3) 0.0489(9) Uani 1 1 d . . . . .
C97 C 0.2344(2) 0.39363(18) 0.8291(3) 0.0567(11) Uani 1 1 d . . . . .
H97 H 0.261354 0.376521 0.860831 0.068 Uiso 1 1 calc R U . . .
C98 C 0.2316(2) 0.43951(19) 0.8417(3) 0.0610(11) Uani 1 1 d . . . . .
H98 H 0.256261 0.453551 0.881815 0.073 Uiso 1 1 calc R U . . .
C99 C 0.1929(2) 0.46499(18) 0.7959(3) 0.0573(11) Uani 1 1 d . . . . .
H99 H 0.191305 0.496576 0.804975 0.069 Uiso 1 1 calc R U . . .
C100 C 0.15618(19) 0.44534(16) 0.7365(3) 0.0497(9) Uani 1 1 d . . . . .
C101 C 0.1995(2) 0.32093(18) 0.7656(4) 0.0592(11) Uani 1 1 d . . . . .
H101 H 0.177320 0.312092 0.714087 0.071 Uiso 1 1 calc R U . . .
C102 C 0.1717(3) 0.3009(2) 0.8372(5) 0.086(2) Uani 1 1 d . . . . .
H10A H 0.191311 0.310978 0.888415 0.129 Uiso 1 1 calc R U . . .
H10B H 0.172556 0.267913 0.834415 0.129 Uiso 1 1 calc R U . . .
H10C H 0.133545 0.311199 0.834167 0.129 Uiso 1 1 calc R U . . .
C103 C 0.2566(2) 0.3009(2) 0.7648(4) 0.0677(14) Uani 1 1 d . . . . .
H10D H 0.275992 0.316495 0.724030 0.101 Uiso 1 1 calc R U . . .
H10E H 0.253629 0.268754 0.751480 0.101 Uiso 1 1 calc R U . . .
H10F H 0.276932 0.304664 0.818296 0.101 Uiso 1 1 calc R U . . .
C104 C 0.1129(2) 0.47351(18) 0.6894(4) 0.0593(10) Uani 1 1 d . . . . .
H104 H 0.093202 0.453729 0.647161 0.071 Uiso 1 1 calc R U . . .
C105 C 0.0710(2) 0.4900(2) 0.7448(5) 0.0819(18) Uani 1 1 d . . . . .
H10G H 0.057336 0.464333 0.774019 0.123 Uiso 1 1 calc R U . . .
H10H H 0.040451 0.504600 0.712250 0.123 Uiso 1 1 calc R U . . .
H10I H 0.088482 0.511754 0.783810 0.123 Uiso 1 1 calc R U . . .
C106 C 0.1383(2) 0.51278(19) 0.6456(4) 0.0659(13) Uani 1 1 d . . . . .
H10J H 0.157875 0.532817 0.685677 0.099 Uiso 1 1 calc R U . . .
H10K H 0.109252 0.529700 0.613962 0.099 Uiso 1 1 calc R U . . .
H10L H 0.164015 0.500858 0.609355 0.099 Uiso 1 1 calc R U . . .
C107 C 0.06917(15) 0.32281(15) 0.4855(3) 0.0392(7) Uani 1 1 d . . . . .
C108 C 0.06804(15) 0.27577(14) 0.4807(3) 0.0374(7) Uani 1 1 d . . . . .
C109 C 0.05289(16) 0.25683(17) 0.4052(3) 0.0453(9) Uani 1 1 d . . . . .
H109 H 0.050847 0.224954 0.399722 0.054 Uiso 1 1 calc R U . . .
C110 C 0.04076(17) 0.28384(19) 0.3378(3) 0.0545(10) Uani 1 1 d . . . . .
H110 H 0.030993 0.270361 0.286463 0.065 Uiso 1 1 calc R U . . .
C111 C 0.04272(18) 0.3302(2) 0.3446(3) 0.0569(10) Uani 1 1 d . . . . .
H111 H 0.034434 0.348225 0.297566 0.068 Uiso 1 1 calc R U . . .
C112 C 0.05653(16) 0.35117(17) 0.4187(3) 0.0487(8) Uani 1 1 d . . . . .
C113 C 0.08301(17) 0.24595(15) 0.5533(3) 0.0433(8) Uani 1 1 d . . . . .
H113 H 0.097213 0.265676 0.599600 0.052 Uiso 1 1 calc R U . . .
C114 C 0.12821(18) 0.21206(17) 0.5379(3) 0.0560(12) Uani 1 1 d . . . . .
H11A H 0.114171 0.190715 0.495682 0.084 Uiso 1 1 calc R U . . .
H11B H 0.139556 0.195582 0.587980 0.084 Uiso 1 1 calc R U . . .
H11C H 0.159732 0.228262 0.520141 0.084 Uiso 1 1 calc R U . . .
C115 C 0.03339(19) 0.22019(18) 0.5783(3) 0.0569(12) Uani 1 1 d . . . . .
H11D H 0.004936 0.241664 0.590392 0.085 Uiso 1 1 calc R U . . .
H11E H 0.044442 0.202062 0.626604 0.085 Uiso 1 1 calc R U . . .
H11F H 0.018977 0.200320 0.533973 0.085 Uiso 1 1 calc R U . . .
C116 C 0.05733(19) 0.40236(18) 0.4252(4) 0.0665(12) Uani 1 1 d D . . . .
H11G H 0.069731 0.406729 0.483966 0.080 Uiso 0.533(17) 1 calc R U P E 2
H116 H 0.088950 0.411834 0.464297 0.080 Uiso 0.467(17) 1 calc R U P E 1
C117 C 0.0005(4) 0.4227(6) 0.4194(9) 0.052(3) Uani 0.533(17) 1 d D . P E 2
H11H H -0.014567 0.424024 0.362404 0.078 Uiso 0.533(17) 1 calc R U P E 2
H11I H 0.002494 0.453248 0.442076 0.078 Uiso 0.533(17) 1 calc R U P E 2
H11J H -0.023271 0.404026 0.449813 0.078 Uiso 0.533(17) 1 calc R U P E 2
C118 C 0.0659(6) 0.4213(4) 0.3372(8) 0.075(4) Uani 0.467(17) 1 d D . P E 1
H11K H 0.095082 0.404247 0.314787 0.113 Uiso 0.467(17) 1 calc R U P E 1
H11L H 0.076028 0.453242 0.341214 0.113 Uiso 0.467(17) 1 calc R U P E 1
H11M H 0.031712 0.418001 0.301606 0.113 Uiso 0.467(17) 1 calc R U P E 1
C122 C 0.0980(5) 0.4277(4) 0.3875(10) 0.076(4) Uani 0.533(17) 1 d D . P E 2
H12A H 0.134636 0.416720 0.407405 0.114 Uiso 0.533(17) 1 calc R U P E 2
H12B H 0.094936 0.459690 0.400970 0.114 Uiso 0.533(17) 1 calc R U P E 2
H12C H 0.092207 0.423781 0.328635 0.114 Uiso 0.533(17) 1 calc R U P E 2
C121 C 0.0075(6) 0.4205(8) 0.4509(11) 0.066(4) Uani 0.467(17) 1 d D . P E 1
H12D H -0.023950 0.408073 0.416906 0.099 Uiso 0.467(17) 1 calc R U P E 1
H12E H 0.007726 0.453388 0.445647 0.099 Uiso 0.467(17) 1 calc R U P E 1
H12F H 0.004789 0.412263 0.507567 0.099 Uiso 0.467(17) 1 calc R U P E 1
C124 C 0.4421(7) 0.4121(6) 0.6143(13) 0.043(5) Uani 0.224(17) 1 d D . P D 2
H12G H 0.474629 0.398028 0.643003 0.064 Uiso 0.224(17) 1 calc R U P D 2
H12H H 0.443886 0.444856 0.622353 0.064 Uiso 0.224(17) 1 calc R U P D 2
H12I H 0.440803 0.405317 0.556363 0.064 Uiso 0.224(17) 1 calc R U P D 2
C123 C 0.3804(14) 0.4159(14) 0.7244(15) 0.074(8) Uani 0.224(17) 1 d D . P D 2
H12J H 0.351946 0.398179 0.747349 0.110 Uiso 0.224(17) 1 calc R U P D 2
H12K H 0.367259 0.446780 0.714168 0.110 Uiso 0.224(17) 1 calc R U P D 2
H12L H 0.413505 0.416467 0.762800 0.110 Uiso 0.224(17) 1 calc R U P D 2
Cl7 Cl 0.4336(3) 0.5463(2) 0.6669(6) 0.0905(18) Uani 0.70(3) 1 d D U P B 2
Cl8 Cl 0.4864(5) 0.5753(3) 0.5271(4) 0.109(2) Uani 0.70(3) 1 d D U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl3 C119 1.785(12) . ?
Cl4 C119 1.756(11) . ?
C119 Cl7 1.741(6) . ?
C119 Cl8 1.758(8) . ?
Cl5 C120 1.759(6) . ?
Cl6 C120 1.759(6) . ?
O1 C5 1.224(5) . ?
O2 C6 1.204(5) . ?
N1 C1 1.357(5) . ?
N1 C2 1.395(5) . ?
N1 C11 1.451(5) . ?
N2 C1 1.353(5) . ?
N2 C3 1.378(5) . ?
N2 C23 1.453(5) . ?
N3 C8 1.341(5) . ?
N3 C9 1.387(5) . ?
N3 C35 1.443(5) . ?
N4 C8 1.349(5) . ?
N4 C10 1.383(5) . ?
N4 C47 1.448(5) . ?
C1 C4 1.433(5) . ?
C2 C3 1.325(6) . ?
C4 C5 1.426(5) . ?
C4 C6 1.456(5) . ?
C5 C7 1.552(5) . ?
C6 C7 1.553(6) . ?
C7 C8 1.478(5) . ?
C9 C10 1.335(6) . ?
C11 C12 1.406(6) . ?
C11 C16 1.401(5) . ?
C12 C13 1.394(5) . ?
C12 C17 1.519(5) . ?
C13 C14 1.377(6) . ?
C14 C15 1.373(6) . ?
C15 C16 1.400(6) . ?
C16 C20 1.509(6) . ?
C17 C18 1.530(6) . ?
C17 C19 1.533(6) . ?
C20 C21 1.528(7) . ?
C20 C22 1.530(6) . ?
C23 C24 1.394(6) . ?
C23 C28 1.382(6) . ?
C24 C25 1.400(6) . ?
C24 C29 1.495(6) . ?
C25 C26 1.372(7) . ?
C26 C27 1.380(7) . ?
C27 C28 1.388(6) . ?
C28 C32 1.532(6) . ?
C29 C30 1.525(6) . ?
C29 C31 1.531(6) . ?
C32 C33 1.546(7) . ?
C32 C34 1.526(7) . ?
C35 C36 1.400(6) . ?
C35 C40 1.387(6) . ?
C36 C37 1.386(6) . ?
C36 C41 1.528(6) . ?
C37 C38 1.353(7) . ?
C38 C39 1.381(7) . ?
C39 C40 1.381(6) . ?
C40 C44 1.537(6) . ?
C41 C42 1.531(6) . ?
C41 C43 1.531(6) . ?
C44 C45 1.530(6) . ?
C44 C46 1.532(7) . ?
C47 C48 1.379(6) . ?
C47 C52 1.418(6) . ?
C48 C49 1.391(6) . ?
C48 C53 1.529(6) . ?
C49 C50 1.384(6) . ?
C50 C51 1.379(7) . ?
C51 C52 1.406(6) . ?
C52 C56 1.509(7) . ?
C53 C54 1.527(6) . ?
C53 C55 1.527(6) . ?
C56 C57 1.532(6) . ?
C56 C58 1.533(7) . ?
O3 C63 1.203(8) . ?
O4 C64 1.210(7) . ?
O5 C66 1.22(3) . ?
O6 C65 1.23(2) . ?
N5 C59 1.346(5) . ?
N5 C60 1.380(5) . ?
N5 C71 1.448(5) . ?
N6 C59 1.342(5) . ?
N6 C61 1.374(5) . ?
N6 C83 1.453(5) . ?
N7 C68 1.346(6) . ?
N7 C69 1.387(5) . ?
N7 C95 1.452(6) . ?
N8 C68 1.352(5) . ?
N8 C70 1.384(5) . ?
N8 C107 1.437(6) . ?
C59 C62 1.469(5) . ?
C60 C61 1.340(6) . ?
C62 C63 1.549(7) . ?
C62 C64 1.537(7) . ?
C62 C65 1.308(19) . ?
C62 C66 1.60(2) . ?
C63 C67 1.480(7) . ?
C64 C67 1.410(7) . ?
C65 C67 1.64(2) . ?
C66 C67 1.38(2) . ?
C67 C68 1.435(5) . ?
C69 C70 1.345(7) . ?
C71 C72 1.394(6) . ?
C71 C76 1.407(6) . ?
C72 C73 1.388(6) . ?
C72 C77 1.516(6) . ?
C73 C74 1.386(6) . ?
C74 C75 1.379(7) . ?
C75 C76 1.400(6) . ?
C76 C80 1.513(7) . ?
C77 C78 1.521(7) . ?
C77 C79 1.521(6) . ?
C80 C81 1.541(8) . ?
C80 C82 1.498(9) . ?
C80 C124 1.443(13) . ?
C80 C123 1.513(14) . ?
C83 C84 1.392(7) . ?
C83 C88 1.386(7) . ?
C84 C85 1.385(6) . ?
C84 C89 1.517(7) . ?
C85 C86 1.370(7) . ?
C86 C87 1.387(7) . ?
C87 C88 1.397(7) . ?
C88 C92 1.532(7) . ?
C89 C90 1.543(7) . ?
C89 C91 1.535(7) . ?
C92 C93 1.531(7) . ?
C92 C94 1.516(8) . ?
C95 C96 1.398(7) . ?
C95 C100 1.390(7) . ?
C96 C97 1.382(7) . ?
C96 C101 1.511(7) . ?
C97 C98 1.379(8) . ?
C98 C99 1.379(8) . ?
C99 C100 1.394(7) . ?
C100 C104 1.506(7) . ?
C101 C102 1.546(8) . ?
C101 C103 1.522(7) . ?
C104 C105 1.525(8) . ?
C104 C106 1.537(8) . ?
C107 C108 1.397(6) . ?
C107 C112 1.400(6) . ?
C108 C109 1.389(6) . ?
C108 C113 1.508(6) . ?
C109 C110 1.382(7) . ?
C110 C111 1.381(8) . ?
C111 C112 1.388(7) . ?
C112 C116 1.521(7) . ?
C113 C114 1.536(6) . ?
C113 C115 1.529(6) . ?
C116 C117 1.513(9) . ?
C116 C118 1.597(11) . ?
C116 C122 1.440(10) . ?
C116 C121 1.437(11) . ?

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
Cl4 C119 Cl3 106.9(8) . . ?
Cl7 C119 Cl8 111.8(5) . . ?
Cl6 C120 Cl5 111.9(3) . . ?
C1 N1 C2 108.7(3) . . ?
C1 N1 C11 128.6(3) . . ?
C2 N1 C11 121.1(3) . . ?
C1 N2 C3 109.8(3) . . ?
C1 N2 C23 127.8(3) . . ?
C3 N2 C23 122.2(3) . . ?
C8 N3 C9 109.1(3) . . ?
C8 N3 C35 128.6(3) . . ?
C9 N3 C35 122.0(3) . . ?
C8 N4 C10 109.4(3) . . ?
C8 N4 C47 126.4(3) . . ?
C10 N4 C47 124.0(3) . . ?
N1 C1 C4 127.7(3) . . ?
N2 C1 N1 106.2(3) . . ?
N2 C1 C4 125.7(3) . . ?
C3 C2 N1 107.8(3) . . ?
C2 C3 N2 107.5(3) . . ?
C1 C4 C6 132.2(4) . . ?
C5 C4 C1 133.2(3) . . ?
C5 C4 C6 92.0(3) . . ?
O1 C5 C4 137.3(3) . . ?
O1 C5 C7 130.3(3) . . ?
C4 C5 C7 92.4(3) . . ?
O2 C6 C4 140.1(4) . . ?
O2 C6 C7 128.6(3) . . ?
C4 C6 C7 91.2(3) . . ?
C5 C7 C6 83.8(3) . . ?
C8 C7 C5 125.2(3) . . ?
C8 C7 C6 124.3(3) . . ?
N3 C8 N4 106.9(3) . . ?
N3 C8 C7 130.5(3) . . ?
N4 C8 C7 122.6(3) . . ?
C10 C9 N3 107.7(3) . . ?
C9 C10 N4 107.0(3) . . ?
C12 C11 N1 119.2(3) . . ?
C16 C11 N1 116.9(3) . . ?
C16 C11 C12 123.5(3) . . ?
C11 C12 C17 122.0(3) . . ?
C13 C12 C11 117.0(3) . . ?
C13 C12 C17 120.9(4) . . ?
C14 C13 C12 121.0(4) . . ?
C15 C14 C13 120.5(4) . . ?
C14 C15 C16 121.9(4) . . ?
C11 C16 C20 122.7(4) . . ?
C15 C16 C11 116.0(4) . . ?
C15 C16 C20 121.2(4) . . ?
C12 C17 C18 112.2(3) . . ?
C12 C17 C19 109.9(3) . . ?
C18 C17 C19 110.1(4) . . ?
C16 C20 C21 112.9(4) . . ?
C16 C20 C22 111.4(4) . . ?
C21 C20 C22 109.8(4) . . ?
C24 C23 N2 118.0(4) . . ?
C28 C23 N2 118.2(3) . . ?
C28 C23 C24 123.5(4) . . ?
C23 C24 C25 116.1(4) . . ?
C23 C24 C29 122.9(4) . . ?
C25 C24 C29 120.9(4) . . ?
C26 C25 C24 122.1(4) . . ?
C25 C26 C27 119.4(4) . . ?
C26 C27 C28 121.4(4) . . ?
C23 C28 C27 117.5(4) . . ?
C23 C28 C32 122.6(4) . . ?
C27 C28 C32 119.8(4) . . ?
C24 C29 C30 112.3(4) . . ?
C24 C29 C31 110.6(4) . . ?
C30 C29 C31 111.2(4) . . ?
C28 C32 C33 109.8(4) . . ?
C34 C32 C28 112.9(5) . . ?
C34 C32 C33 111.9(5) . . ?
C36 C35 N3 118.2(4) . . ?
C40 C35 N3 118.1(3) . . ?
C40 C35 C36 123.3(4) . . ?
C35 C36 C41 122.3(4) . . ?
C37 C36 C35 116.3(4) . . ?
C37 C36 C41 121.3(4) . . ?
C38 C37 C36 121.7(4) . . ?
C37 C38 C39 120.7(4) . . ?
C40 C39 C38 120.8(4) . . ?
C35 C40 C44 122.0(4) . . ?
C39 C40 C35 117.2(4) . . ?
C39 C40 C44 120.8(4) . . ?
C36 C41 C42 109.8(4) . . ?
C36 C41 C43 111.6(3) . . ?
C43 C41 C42 111.1(4) . . ?
C45 C44 C40 111.0(4) . . ?
C45 C44 C46 109.1(4) . . ?
C46 C44 C40 112.9(4) . . ?
C48 C47 N4 119.1(3) . . ?
C48 C47 C52 123.9(4) . . ?
C52 C47 N4 117.0(4) . . ?
C47 C48 C49 118.1(4) . . ?
C47 C48 C53 122.4(4) . . ?
C49 C48 C53 119.5(4) . . ?
C50 C49 C48 120.7(4) . . ?
C51 C50 C49 119.9(4) . . ?
C50 C51 C52 122.5(4) . . ?
C47 C52 C56 122.4(4) . . ?
C51 C52 C47 114.8(4) . . ?
C51 C52 C56 122.7(4) . . ?
C54 C53 C48 110.2(4) . . ?
C54 C53 C55 111.4(4) . . ?
C55 C53 C48 111.1(3) . . ?
C52 C56 C57 111.5(4) . . ?
C52 C56 C58 112.5(4) . . ?
C57 C56 C58 108.9(4) . . ?
C59 N5 C60 109.4(3) . . ?
C59 N5 C71 125.3(3) . . ?
C60 N5 C71 125.3(3) . . ?
C59 N6 C61 109.5(3) . . ?
C59 N6 C83 128.5(3) . . ?
C61 N6 C83 122.0(3) . . ?
C68 N7 C69 110.1(3) . . ?
C68 N7 C95 127.2(3) . . ?
C69 N7 C95 122.6(4) . . ?
C68 N8 C70 109.1(4) . . ?
C68 N8 C107 126.9(3) . . ?
C70 N8 C107 124.0(3) . . ?
N5 C59 C62 122.5(4) . . ?
N6 C59 N5 106.7(3) . . ?
N6 C59 C62 130.5(3) . . ?
C61 C60 N5 107.0(3) . . ?
C60 C61 N6 107.5(4) . . ?
C59 C62 C63 131.2(4) . . ?
C59 C62 C64 125.9(4) . . ?
C59 C62 C66 120.4(9) . . ?
C64 C62 C63 85.4(4) . . ?
C65 C62 C59 134.6(9) . . ?
C65 C62 C66 90.4(12) . . ?
O3 C63 C62 132.5(5) . . ?
O3 C63 C67 138.4(5) . . ?
C67 C63 C62 89.1(4) . . ?
O4 C64 C62 130.7(5) . . ?
O4 C64 C67 137.1(5) . . ?
C67 C64 C62 92.2(4) . . ?
O6 C65 C62 132.3(16) . . ?
O6 C65 C67 134.8(14) . . ?
C62 C65 C67 91.6(12) . . ?
O5 C66 C62 144.0(18) . . ?
O5 C66 C67 124.7(17) . . ?
C67 C66 C62 90.9(13) . . ?
C64 C67 C63 92.7(4) . . ?
C64 C67 C68 133.0(4) . . ?
C66 C67 C65 86.3(12) . . ?
C66 C67 C68 141.2(10) . . ?
C68 C67 C63 130.5(4) . . ?
C68 C67 C65 129.8(8) . . ?
N7 C68 N8 106.5(3) . . ?
N7 C68 C67 126.4(4) . . ?
N8 C68 C67 127.0(4) . . ?
C70 C69 N7 106.3(4) . . ?
C69 C70 N8 107.9(3) . . ?
C72 C71 N5 118.6(4) . . ?
C72 C71 C76 123.9(4) . . ?
C76 C71 N5 117.4(4) . . ?
C71 C72 C77 123.1(4) . . ?
C73 C72 C71 116.9(4) . . ?
C73 C72 C77 120.0(4) . . ?
C74 C73 C72 121.2(4) . . ?
C75 C74 C73 120.5(4) . . ?
C74 C75 C76 121.2(4) . . ?
C71 C76 C80 123.0(4) . . ?
C75 C76 C71 116.2(4) . . ?
C75 C76 C80 120.7(4) . . ?
C72 C77 C78 111.8(4) . . ?
C72 C77 C79 110.5(4) . . ?
C79 C77 C78 110.5(4) . . ?
C76 C80 C81 112.0(5) . . ?
C76 C80 C123 113.3(17) . . ?
C82 C80 C76 113.7(7) . . ?
C82 C80 C81 109.3(6) . . ?
C124 C80 C76 114.2(8) . . ?
C124 C80 C123 114.7(13) . . ?
C84 C83 N6 117.4(4) . . ?
C88 C83 N6 118.2(4) . . ?
C88 C83 C84 123.9(4) . . ?
C83 C84 C89 123.2(4) . . ?
C85 C84 C83 116.4(4) . . ?
C85 C84 C89 120.4(4) . . ?
C86 C85 C84 121.4(5) . . ?
C85 C86 C87 121.2(5) . . ?
C86 C87 C88 119.4(5) . . ?
C83 C88 C87 117.6(5) . . ?
C83 C88 C92 123.4(4) . . ?
C87 C88 C92 118.9(5) . . ?
C84 C89 C90 111.8(4) . . ?
C84 C89 C91 110.5(4) . . ?
C91 C89 C90 110.0(5) . . ?
C93 C92 C88 109.3(4) . . ?
C94 C92 C88 114.7(4) . . ?
C94 C92 C93 110.4(5) . . ?
C96 C95 N7 117.7(4) . . ?
C100 C95 N7 117.9(4) . . ?
C100 C95 C96 124.3(4) . . ?
C95 C96 C101 123.1(4) . . ?
C97 C96 C95 116.1(5) . . ?
C97 C96 C101 120.4(5) . . ?
C98 C97 C96 122.0(5) . . ?
C97 C98 C99 119.9(5) . . ?
C98 C99 C100 121.4(5) . . ?
C95 C100 C99 116.3(5) . . ?
C95 C100 C104 123.2(4) . . ?
C99 C100 C104 120.4(5) . . ?
C96 C101 C102 108.9(5) . . ?
C96 C101 C103 113.7(4) . . ?
C103 C101 C102 109.5(5) . . ?
C100 C104 C105 110.3(5) . . ?
C100 C104 C106 111.5(4) . . ?
C105 C104 C106 111.8(5) . . ?
C108 C107 N8 117.4(4) . . ?
C108 C107 C112 123.6(4) . . ?
C112 C107 N8 118.9(4) . . ?
C107 C108 C113 122.6(4) . . ?
C109 C108 C107 117.1(4) . . ?
C109 C108 C113 120.3(4) . . ?
C110 C109 C108 120.7(5) . . ?
C111 C110 C109 120.6(5) . . ?
C110 C111 C112 121.4(5) . . ?
C107 C112 C116 122.8(5) . . ?
C111 C112 C107 116.6(5) . . ?
C111 C112 C116 120.6(5) . . ?
C108 C113 C114 111.9(4) . . ?
C108 C113 C115 111.9(4) . . ?
C115 C113 C114 109.0(4) . . ?
C112 C116 C118 106.7(7) . . ?
C117 C116 C112 112.8(8) . . ?
C122 C116 C112 119.6(7) . . ?
C122 C116 C117 116.0(8) . . ?
C121 C116 C112 112.8(11) . . ?
C121 C116 C118 109.4(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C5 C7 C6 -174.8(4) . . . . ?
O1 C5 C7 C8 -46.8(6) . . . . ?
O2 C6 C7 C5 176.1(4) . . . . ?
O2 C6 C7 C8 47.3(6) . . . . ?
N1 C1 C4 C5 24.3(7) . . . . ?
N1 C1 C4 C6 -179.5(4) . . . . ?
N1 C2 C3 N2 -0.1(4) . . . . ?
N1 C11 C12 C13 -173.3(3) . . . . ?
N1 C11 C12 C17 3.7(5) . . . . ?
N1 C11 C16 C15 174.9(3) . . . . ?
N1 C11 C16 C20 -2.5(5) . . . . ?
N2 C1 C4 C5 -147.2(4) . . . . ?
N2 C1 C4 C6 9.1(7) . . . . ?
N2 C23 C24 C25 175.1(3) . . . . ?
N2 C23 C24 C29 -2.7(6) . . . . ?
N2 C23 C28 C27 -175.6(4) . . . . ?
N2 C23 C28 C32 7.4(6) . . . . ?
N3 C9 C10 N4 0.0(5) . . . . ?
N3 C35 C36 C37 172.6(3) . . . . ?
N3 C35 C36 C41 -5.0(6) . . . . ?
N3 C35 C40 C39 -174.3(3) . . . . ?
N3 C35 C40 C44 2.5(6) . . . . ?
N4 C47 C48 C49 -175.1(3) . . . . ?
N4 C47 C48 C53 5.0(5) . . . . ?
N4 C47 C52 C51 176.7(3) . . . . ?
N4 C47 C52 C56 -2.2(5) . . . . ?
C1 N1 C2 C3 -0.6(4) . . . . ?
C1 N1 C11 C12 -109.9(4) . . . . ?
C1 N1 C11 C16 76.3(5) . . . . ?
C1 N2 C3 C2 0.8(4) . . . . ?
C1 N2 C23 C24 92.9(5) . . . . ?
C1 N2 C23 C28 -93.0(5) . . . . ?
C1 C4 C5 O1 -22.9(8) . . . . ?
C1 C4 C5 C7 156.9(4) . . . . ?
C1 C4 C6 O2 21.1(9) . . . . ?
C1 C4 C6 C7 -157.2(4) . . . . ?
C2 N1 C1 N2 1.1(4) . . . . ?
C2 N1 C1 C4 -171.7(4) . . . . ?
C2 N1 C11 C12 86.0(4) . . . . ?
C2 N1 C11 C16 -87.7(4) . . . . ?
C3 N2 C1 N1 -1.2(4) . . . . ?
C3 N2 C1 C4 171.8(4) . . . . ?
C3 N2 C23 C24 -92.9(4) . . . . ?
C3 N2 C23 C28 81.2(5) . . . . ?
C4 C5 C7 C6 5.4(3) . . . . ?
C4 C5 C7 C8 133.4(4) . . . . ?
C4 C6 C7 C5 -5.3(3) . . . . ?
C4 C6 C7 C8 -134.1(4) . . . . ?
C5 C4 C6 O2 -176.0(6) . . . . ?
C5 C4 C6 C7 5.7(3) . . . . ?
C5 C7 C8 N3 -60.5(6) . . . . ?
C5 C7 C8 N4 119.2(4) . . . . ?
C6 C4 C5 O1 174.5(5) . . . . ?
C6 C4 C5 C7 -5.7(3) . . . . ?
C6 C7 C8 N3 48.1(6) . . . . ?
C6 C7 C8 N4 -132.1(4) . . . . ?
C8 N3 C9 C10 0.5(4) . . . . ?
C8 N3 C35 C36 99.4(5) . . . . ?
C8 N3 C35 C40 -88.4(5) . . . . ?
C8 N4 C10 C9 -0.5(5) . . . . ?
C8 N4 C47 C48 -106.8(4) . . . . ?
C8 N4 C47 C52 75.8(5) . . . . ?
C9 N3 C8 N4 -0.8(4) . . . . ?
C9 N3 C8 C7 179.0(4) . . . . ?
C9 N3 C35 C36 -88.7(5) . . . . ?
C9 N3 C35 C40 83.6(5) . . . . ?
C10 N4 C8 N3 0.8(4) . . . . ?
C10 N4 C8 C7 -179.0(3) . . . . ?
C10 N4 C47 C48 79.0(5) . . . . ?
C10 N4 C47 C52 -98.4(4) . . . . ?
C11 N1 C1 N2 -164.5(3) . . . . ?
C11 N1 C1 C4 22.7(6) . . . . ?
C11 N1 C2 C3 166.3(4) . . . . ?
C11 C12 C13 C14 -0.9(5) . . . . ?
C11 C12 C17 C18 134.7(4) . . . . ?
C11 C12 C17 C19 -102.4(4) . . . . ?
C11 C16 C20 C21 -141.1(4) . . . . ?
C11 C16 C20 C22 94.9(4) . . . . ?
C12 C11 C16 C15 1.4(5) . . . . ?
C12 C11 C16 C20 -176.0(3) . . . . ?
C12 C13 C14 C15 0.3(5) . . . . ?
C13 C12 C17 C18 -48.4(5) . . . . ?
C13 C12 C17 C19 74.5(4) . . . . ?
C13 C14 C15 C16 1.3(6) . . . . ?
C14 C15 C16 C11 -2.0(5) . . . . ?
C14 C15 C16 C20 175.4(4) . . . . ?
C15 C16 C20 C21 41.6(5) . . . . ?
C15 C16 C20 C22 -82.4(5) . . . . ?
C16 C11 C12 C13 0.0(5) . . . . ?
C16 C11 C12 C17 177.0(3) . . . . ?
C17 C12 C13 C14 -178.0(3) . . . . ?
C23 N2 C1 N1 173.6(3) . . . . ?
C23 N2 C1 C4 -13.5(6) . . . . ?
C23 N2 C3 C2 -174.3(4) . . . . ?
C23 C24 C25 C26 -1.2(6) . . . . ?
C23 C24 C29 C30 -123.7(4) . . . . ?
C23 C24 C29 C31 111.5(4) . . . . ?
C23 C28 C32 C33 97.0(5) . . . . ?
C23 C28 C32 C34 -137.4(5) . . . . ?
C24 C23 C28 C27 -1.9(6) . . . . ?
C24 C23 C28 C32 -178.9(4) . . . . ?
C24 C25 C26 C27 1.6(7) . . . . ?
C25 C24 C29 C30 58.6(5) . . . . ?
C25 C24 C29 C31 -66.2(5) . . . . ?
C25 C26 C27 C28 -2.2(7) . . . . ?
C26 C27 C28 C23 2.3(6) . . . . ?
C26 C27 C28 C32 179.4(4) . . . . ?
C27 C28 C32 C33 -79.9(5) . . . . ?
C27 C28 C32 C34 45.7(7) . . . . ?
C28 C23 C24 C25 1.4(6) . . . . ?
C28 C23 C24 C29 -176.4(4) . . . . ?
C29 C24 C25 C26 176.7(4) . . . . ?
C35 N3 C8 N4 172.0(4) . . . . ?
C35 N3 C8 C7 -8.2(7) . . . . ?
C35 N3 C9 C10 -172.9(4) . . . . ?
C35 C36 C37 C38 0.9(6) . . . . ?
C35 C36 C41 C42 105.3(5) . . . . ?
C35 C36 C41 C43 -131.0(4) . . . . ?
C35 C40 C44 C45 -92.9(5) . . . . ?
C35 C40 C44 C46 144.2(4) . . . . ?
C36 C35 C40 C39 -2.5(6) . . . . ?
C36 C35 C40 C44 174.4(4) . . . . ?
C36 C37 C38 C39 -0.9(7) . . . . ?
C37 C36 C41 C42 -72.2(5) . . . . ?
C37 C36 C41 C43 51.5(5) . . . . ?
C37 C38 C39 C40 -0.8(7) . . . . ?
C38 C39 C40 C35 2.4(6) . . . . ?
C38 C39 C40 C44 -174.4(4) . . . . ?
C39 C40 C44 C45 83.8(5) . . . . ?
C39 C40 C44 C46 -39.1(6) . . . . ?
C40 C35 C36 C37 0.8(6) . . . . ?
C40 C35 C36 C41 -176.8(4) . . . . ?
C41 C36 C37 C38 178.6(4) . . . . ?
C47 N4 C8 N3 -174.1(4) . . . . ?
C47 N4 C8 C7 6.1(6) . . . . ?
C47 N4 C10 C9 174.5(4) . . . . ?
C47 C48 C49 C50 -1.5(5) . . . . ?
C47 C48 C53 C54 118.7(4) . . . . ?
C47 C48 C53 C55 -117.3(5) . . . . ?
C47 C52 C56 C57 80.9(5) . . . . ?
C47 C52 C56 C58 -156.3(4) . . . . ?
C48 C47 C52 C51 -0.6(5) . . . . ?
C48 C47 C52 C56 -179.6(4) . . . . ?
C48 C49 C50 C51 -0.6(6) . . . . ?
C49 C48 C53 C54 -61.1(5) . . . . ?
C49 C48 C53 C55 62.9(5) . . . . ?
C49 C50 C51 C52 2.3(6) . . . . ?
C50 C51 C52 C47 -1.6(6) . . . . ?
C50 C51 C52 C56 177.3(4) . . . . ?
C51 C52 C56 C57 -97.9(5) . . . . ?
C51 C52 C56 C58 24.8(5) . . . . ?
C52 C47 C48 C49 2.2(5) . . . . ?
C52 C47 C48 C53 -177.7(3) . . . . ?
C53 C48 C49 C50 178.3(4) . . . . ?
O3 C63 C67 C64 170.9(9) . . . . ?
O3 C63 C67 C68 -29.4(12) . . . . ?
O4 C64 C67 C63 -172.9(8) . . . . ?
O4 C64 C67 C68 28.2(12) . . . . ?
O5 C66 C67 C65 180(3) . . . . ?
O5 C66 C67 C68 -19(4) . . . . ?
O6 C65 C67 C66 175(3) . . . . ?
O6 C65 C67 C68 10(3) . . . . ?
N5 C59 C62 C63 133.3(5) . . . . ?
N5 C59 C62 C64 -106.7(5) . . . . ?
N5 C59 C62 C65 -72.6(15) . . . . ?
N5 C59 C62 C66 161.4(11) . . . . ?
N5 C60 C61 N6 0.1(5) . . . . ?
N5 C71 C72 C73 179.5(3) . . . . ?
N5 C71 C72 C77 -0.4(5) . . . . ?
N5 C71 C76 C75 179.8(3) . . . . ?
N5 C71 C76 C80 -0.5(5) . . . . ?
N6 C59 C62 C63 -53.3(7) . . . . ?
N6 C59 C62 C64 66.7(7) . . . . ?
N6 C59 C62 C65 100.8(15) . . . . ?
N6 C59 C62 C66 -25.2(12) . . . . ?
N6 C83 C84 C85 -172.1(4) . . . . ?
N6 C83 C84 C89 6.7(6) . . . . ?
N6 C83 C88 C87 173.0(4) . . . . ?
N6 C83 C88 C92 -3.4(6) . . . . ?
N7 C69 C70 N8 -0.3(5) . . . . ?
N7 C95 C96 C97 -176.6(4) . . . . ?
N7 C95 C96 C101 -3.0(6) . . . . ?
N7 C95 C100 C99 176.2(4) . . . . ?
N7 C95 C100 C104 -0.6(7) . . . . ?
N8 C107 C108 C109 175.6(3) . . . . ?
N8 C107 C108 C113 -5.1(5) . . . . ?
N8 C107 C112 C111 -176.7(4) . . . . ?
N8 C107 C112 C116 3.0(6) . . . . ?
C59 N5 C60 C61 0.4(5) . . . . ?
C59 N5 C71 C72 103.2(4) . . . . ?
C59 N5 C71 C76 -77.6(5) . . . . ?
C59 N6 C61 C60 -0.6(5) . . . . ?
C59 N6 C83 C84 -101.2(5) . . . . ?
C59 N6 C83 C88 86.5(6) . . . . ?
C59 C62 C63 O3 -36.4(11) . . . . ?
C59 C62 C63 C67 141.1(5) . . . . ?
C59 C62 C64 O4 34.1(9) . . . . ?
C59 C62 C64 C67 -145.3(4) . . . . ?
C59 C62 C65 O6 50(3) . . . . ?
C59 C62 C65 C67 -142.2(7) . . . . ?
C59 C62 C66 O5 -36(4) . . . . ?
C59 C62 C66 C67 152.5(7) . . . . ?
C60 N5 C59 N6 -0.7(5) . . . . ?
C60 N5 C59 C62 174.0(4) . . . . ?
C60 N5 C71 C72 -80.6(5) . . . . ?
C60 N5 C71 C76 98.6(5) . . . . ?
C61 N6 C59 N5 0.8(5) . . . . ?
C61 N6 C59 C62 -173.4(4) . . . . ?
C61 N6 C83 C84 79.9(5) . . . . ?
C61 N6 C83 C88 -92.5(5) . . . . ?
C62 C63 C67 C64 -6.4(4) . . . . ?
C62 C63 C67 C68 153.4(5) . . . . ?
C62 C64 C67 C63 6.4(4) . . . . ?
C62 C64 C67 C68 -152.5(5) . . . . ?
C62 C65 C67 C66 7.5(13) . . . . ?
C62 C65 C67 C68 -157.1(6) . . . . ?
C62 C66 C67 C65 -6.1(11) . . . . ?
C62 C66 C67 C68 154.8(9) . . . . ?
C63 C62 C64 O4 173.3(8) . . . . ?
C63 C62 C64 C67 -6.1(4) . . . . ?
C63 C67 C68 N7 -23.3(8) . . . . ?
C63 C67 C68 N8 161.3(5) . . . . ?
C64 C62 C63 O3 -171.7(8) . . . . ?
C64 C62 C63 C67 5.8(4) . . . . ?
C64 C67 C68 N7 128.5(6) . . . . ?
C64 C67 C68 N8 -47.0(8) . . . . ?
C65 C62 C66 O5 179(4) . . . . ?
C65 C62 C66 C67 7.6(14) . . . . ?
C65 C67 C68 N7 94.7(11) . . . . ?
C65 C67 C68 N8 -80.7(11) . . . . ?
C66 C62 C65 O6 -174(3) . . . . ?
C66 C62 C65 C67 -6.4(11) . . . . ?
C66 C67 C68 N7 -60.1(19) . . . . ?
C66 C67 C68 N8 124.5(18) . . . . ?
C68 N7 C69 C70 -0.3(6) . . . . ?
C68 N7 C95 C96 -80.7(6) . . . . ?
C68 N7 C95 C100 101.7(5) . . . . ?
C68 N8 C70 C69 0.7(5) . . . . ?
C68 N8 C107 C108 106.2(5) . . . . ?
C68 N8 C107 C112 -77.3(5) . . . . ?
C69 N7 C68 N8 0.8(5) . . . . ?
C69 N7 C68 C67 -175.4(4) . . . . ?
C69 N7 C95 C96 95.7(5) . . . . ?
C69 N7 C95 C100 -81.8(6) . . . . ?
C70 N8 C68 N7 -0.9(5) . . . . ?
C70 N8 C68 C67 175.2(4) . . . . ?
C70 N8 C107 C108 -73.5(5) . . . . ?
C70 N8 C107 C112 102.9(5) . . . . ?
C71 N5 C59 N6 175.9(4) . . . . ?
C71 N5 C59 C62 -9.3(6) . . . . ?
C71 N5 C60 C61 -176.3(4) . . . . ?
C71 C72 C73 C74 0.4(6) . . . . ?
C71 C72 C77 C78 -127.3(4) . . . . ?
C71 C72 C77 C79 109.2(5) . . . . ?
C71 C76 C80 C81 -119.8(6) . . . . ?
C71 C76 C80 C82 115.7(9) . . . . ?
C71 C76 C80 C124 -81.0(11) . . . . ?
C71 C76 C80 C123 145.2(16) . . . . ?
C72 C71 C76 C75 -1.1(6) . . . . ?
C72 C71 C76 C80 178.6(4) . . . . ?
C72 C73 C74 C75 -0.6(6) . . . . ?
C73 C72 C77 C78 52.7(5) . . . . ?
C73 C72 C77 C79 -70.8(5) . . . . ?
C73 C74 C75 C76 -0.1(6) . . . . ?
C74 C75 C76 C71 0.9(6) . . . . ?
C74 C75 C76 C80 -178.8(4) . . . . ?
C75 C76 C80 C81 59.9(7) . . . . ?
C75 C76 C80 C82 -64.6(9) . . . . ?
C75 C76 C80 C124 98.6(11) . . . . ?
C75 C76 C80 C123 -35.1(16) . . . . ?
C76 C71 C72 C73 0.4(6) . . . . ?
C76 C71 C72 C77 -179.6(4) . . . . ?
C77 C72 C73 C74 -179.6(4) . . . . ?
C83 N6 C59 N5 -178.3(4) . . . . ?
C83 N6 C59 C62 7.5(7) . . . . ?
C83 N6 C61 C60 178.6(4) . . . . ?
C83 C84 C85 C86 -0.3(7) . . . . ?
C83 C84 C89 C90 130.4(5) . . . . ?
C83 C84 C89 C91 -106.7(5) . . . . ?
C83 C88 C92 C93 88.8(6) . . . . ?
C83 C88 C92 C94 -146.6(5) . . . . ?
C84 C83 C88 C87 1.2(7) . . . . ?
C84 C83 C88 C92 -175.3(4) . . . . ?
C84 C85 C86 C87 -0.3(8) . . . . ?
C85 C84 C89 C90 -50.9(6) . . . . ?
C85 C84 C89 C91 72.1(5) . . . . ?
C85 C86 C87 C88 1.3(8) . . . . ?
C86 C87 C88 C83 -1.7(7) . . . . ?
C86 C87 C88 C92 174.9(5) . . . . ?
C87 C88 C92 C93 -87.7(6) . . . . ?
C87 C88 C92 C94 36.9(7) . . . . ?
C88 C83 C84 C85 -0.2(6) . . . . ?
C88 C83 C84 C89 178.6(4) . . . . ?
C89 C84 C85 C86 -179.1(4) . . . . ?
C95 N7 C68 N8 177.6(4) . . . . ?
C95 N7 C68 C67 1.4(7) . . . . ?
C95 N7 C69 C70 -177.3(4) . . . . ?
C95 C96 C97 C98 0.1(7) . . . . ?
C95 C96 C101 C102 -98.9(6) . . . . ?
C95 C96 C101 C103 138.7(5) . . . . ?
C95 C100 C104 C105 109.1(5) . . . . ?
C95 C100 C104 C106 -126.0(5) . . . . ?
C96 C95 C100 C99 -1.2(7) . . . . ?
C96 C95 C100 C104 -177.9(5) . . . . ?
C96 C97 C98 C99 -0.4(8) . . . . ?
C97 C96 C101 C102 74.4(6) . . . . ?
C97 C96 C101 C103 -48.0(7) . . . . ?
C97 C98 C99 C100 0.0(8) . . . . ?
C98 C99 C100 C95 0.8(7) . . . . ?
C98 C99 C100 C104 177.6(5) . . . . ?
C99 C100 C104 C105 -67.5(6) . . . . ?
C99 C100 C104 C106 57.3(7) . . . . ?
C100 C95 C96 C97 0.7(7) . . . . ?
C100 C95 C96 C101 174.3(4) . . . . ?
C101 C96 C97 C98 -173.7(5) . . . . ?
C107 N8 C68 N7 179.3(4) . . . . ?
C107 N8 C68 C67 -4.6(7) . . . . ?
C107 N8 C70 C69 -179.5(4) . . . . ?
C107 C108 C109 C110 1.4(6) . . . . ?
C107 C108 C113 C114 -125.2(4) . . . . ?
C107 C108 C113 C115 112.1(5) . . . . ?
C107 C112 C116 C117 -105.7(8) . . . . ?
C107 C112 C116 C118 156.7(7) . . . . ?
C107 C112 C116 C122 112.5(9) . . . . ?
C107 C112 C116 C121 -83.1(10) . . . . ?
C108 C107 C112 C111 -0.5(6) . . . . ?
C108 C107 C112 C116 179.3(4) . . . . ?
C108 C109 C110 C111 -0.9(6) . . . . ?
C109 C108 C113 C114 54.1(5) . . . . ?
C109 C108 C113 C115 -68.5(5) . . . . ?
C109 C110 C111 C112 -0.3(7) . . . . ?
C110 C111 C112 C107 1.0(6) . . . . ?
C110 C111 C112 C116 -178.7(4) . . . . ?
C111 C112 C116 C117 74.1(8) . . . . ?
C111 C112 C116 C118 -23.5(8) . . . . ?
C111 C112 C116 C122 -67.7(10) . . . . ?
C111 C112 C116 C121 96.7(10) . . . . ?
C112 C107 C108 C109 -0.7(6) . . . . ?
C112 C107 C108 C113 178.7(4) . . . . ?
C113 C108 C109 C110 -178.0(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 318 electrons were 
found in a volume of 1540Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
0.95[CH2Cl2] per Asymmetric Unit 
which account for 319 electrons 
per unit cell.
;
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 0.000 0.000 0.500 738.4 158.9 '3.8 CH2Cl2'
2 0.000 0.500 0.000 738.4 158.9 '3.8 CH2Cl2'
3 0.170 0.567 0.496 15.9 0.0 ?
4 0.170 0.933 -0.004 15.9 0.0 ?
5 0.280 0.620 0.411 7.3 0.0 ?
6 0.280 0.880 0.911 7.3 0.0 ?
7 0.720 0.120 0.089 7.3 0.0 ?
8 0.720 0.380 0.589 7.3 0.0 ?
9 0.830 0.067 0.004 15.9 0.0 ?
10 0.830 0.433 0.504 15.9 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2021-05-27
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.752
_oxdiff_exptl_absorpt_empirical_full_min 0.462
####################################################################### 
# 
# 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_wf446meoh
_database_code_depnum_ccdc_archive 'CCDC 2094754'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-05-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H40 N2 O2'
_chemical_formula_sum            'C30 H40 N2 O2'
_chemical_formula_weight         460.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H40 N2 O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.8074(4)
_cell_length_b                   16.1835(6)
_cell_length_c                   16.6250(7)
_cell_angle_alpha                62.421(4)
_cell_angle_beta                 83.645(3)
_cell_angle_gamma                82.289(3)
_cell_volume                     2786.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10294
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.2860
_cell_measurement_theta_min      6.0140
_shelx_estimated_absorpt_T_max   0.949
_shelx_estimated_absorpt_T_min   0.904
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
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 pale colourless'
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 1 0.0825
-1 -1 2 0.0828
1 0 2 0.0891
-2 -1 -1 0.0661
3 -5 6 0.0791
-3 -7 3 0.0914
3 7 -3 0.1155
-4 7 -1 0.0534
4 -7 1 0.0788
7 5 3 0.0891
4 -8 -4 0.0617
-4 8 7 0.0525
4 -8 -7 0.0473
0 -9 -10 0.0322
-1 5 10 0.0672
-3 5 -5 0.0700
-3 9 3 0.0482
0 0 10 0.0623
0 -10 -5 0.0592
7 -3 -1 0.0581
-1 9 0 0.0623

_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.1
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
2.0004 1.0004 0.9999 0.0147 0.0260 0.2694
-1.0006 -0.9996 2.0005 0.1300 0.2427 -0.1342
1.0000 0.0006 2.0002 0.0811 0.1857 0.1308
-2.0004 -1.0004 -0.9999 -0.0147 -0.0260 -0.2694
2.5687 -4.7823 5.5348 0.0252 0.9713 0.2367
-3.2331 -7.0376 2.8036 0.0214 0.8475 -0.5303
3.1281 7.0339 -2.8808 -0.0217 -0.8556 0.5171
-3.8306 7.2967 -0.6596 0.4529 -0.8337 -0.3158
3.7213 -7.4040 0.6150 -0.4554 0.8382 0.3000
7.1890 4.9308 2.7564 0.0577 -0.1048 0.9928
4.0267 -8.0710 -4.3294 -0.8132 0.4980 0.3011
-3.6837 7.5432 6.9212 0.9393 -0.2252 -0.2589
3.6327 -7.5887 -6.9566 -0.9412 0.2256 0.2516
-0.1898 -8.5132 -9.5407 -0.9691 0.0248 -0.2454
-1.2699 4.7017 10.3745 0.9237 0.3831 -0.0093
-2.9898 5.3452 -4.6367 0.0760 -0.9592 -0.2722
-2.9839 8.9712 2.9473 0.7162 -0.6790 -0.1611
-0.0541 -0.0267 9.5341 0.6080 0.7931 0.0352
0.0161 -10.4064 -4.9749 -0.7705 0.5905 -0.2400
6.8894 -3.2814 -0.7422 -0.5087 0.3906 0.7672
-1.3017 9.1142 0.3165 0.4773 -0.8781 0.0353

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11529
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.806
_diffrn_reflns_theta_min         3.003
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 -48.00   1.00    7.50    --  -43.13 129.00 -90.00   26
  2  ω   -114.00 -67.00   1.00    7.50    --  -43.13-141.00  24.00   47
  3  ω     49.00 101.00   1.00    7.50    --   43.13-129.00-163.00   52
  4  ω     54.00  79.00   1.00    7.50    --   43.13-141.00  24.00   25
  5  ω     96.00 136.00   1.00   30.00    --  103.80 129.00 -90.00   40
  6  ω     65.00 113.00   1.00   30.00    --  103.80-129.00-163.00   48
  7  ω    106.00 131.00   1.00   30.00    --  103.80 141.00  81.00   25
  8  ω     71.00 125.00   1.00   30.00    --  103.80-141.00  24.00   54
  9  ω     37.00  62.00   1.00   30.00    --  103.80-141.00  24.00   25
 10  ω    -66.00 -41.00   1.00    7.50    --  -43.13 141.00  81.00   25
 11  ω    -66.00  30.00   1.00    7.50    --  -43.13  37.00  30.00   96
 12  ω   -117.00 -19.00   1.00    7.50    --  -43.13 -37.00  30.00   98
 13  ω     20.00 118.00   1.00    7.50    --   43.13  37.00 -90.00   98
 14  ω    -10.00  15.00   1.00    7.50    --   43.13 -77.00  90.00   25
 15  ω     41.00 104.00   1.00   30.00    --  103.80-111.00-120.00   63
 16  ω    152.00 177.00   1.00   30.00    --  103.80  30.00 -90.00   25
 17  ω    107.00 171.00   1.00   30.00    --  103.80 111.00 150.00   64
 18  ω     83.00 138.00   1.00   30.00    --  103.80  30.00 -90.00   55
 19  ω     28.00 112.00   1.00   30.00    --  103.80 -30.00-120.00   84
 20  ω     40.00 121.00   1.00   30.00    --  103.80 -30.00  30.00   81
 21  ω     39.00 106.00   1.00   30.00    --  103.80-111.00  90.00   67
 22  ω     35.00  60.00   1.00   30.00    --  103.80 -77.00   0.00   25
 23  ω    103.00 132.00   1.00   30.00    --  103.80 -77.00   0.00   29
 24  ω     63.00 112.00   1.00   30.00    --  103.80 -45.00-180.00   49
 25  ω    106.00 166.00   1.00   30.00    --  103.80 111.00 -60.00   60
 26  ω     78.00 105.00   1.00   30.00    --  103.80-111.00   0.00   27
 27  ω    105.00 178.00   1.00   30.00    --  103.80 111.00  30.00   73
 28  ω     85.00 176.00   1.00   30.00    --  103.80  45.00-150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0462452000
_diffrn_orient_matrix_UB_12      0.0435493000
_diffrn_orient_matrix_UB_13      0.0636352000
_diffrn_orient_matrix_UB_21      0.0197171000
_diffrn_orient_matrix_UB_22      -0.0964071000
_diffrn_orient_matrix_UB_23      0.0830296000
_diffrn_orient_matrix_UB_31      0.1219075000
_diffrn_orient_matrix_UB_32      0.0211270000
_diffrn_orient_matrix_UB_33      0.0044487000
_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                7996
_reflns_number_total             11529
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         11529
_refine_ls_number_restraints     708
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0998P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1521
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.611(2)
 0.389(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C55-C54 \\sim C56-C54 \\sim C57-C54 \\sim C58-C54
 with sigma of 0.02
 C55-C57 \\sim C56-C58
 with sigma of 0.02
 C26-C27 \\sim C28-C29
 with sigma of 0.02
 C26-C25 \\sim C28-C25 \\sim C27-C25 \\sim C29-C25
 with sigma of 0.02
 C60-C59 \\sim C62-C59 \\sim C61-C59 \\sim C63-C59
 with sigma of 0.02
 C60-C61 \\sim C62-C63
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H54A)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C57)=Sof(H57A)=Sof(H57B)=
 Sof(H57C)=1-FVAR(1)
 Sof(H54)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C58)=Sof(H58A)=Sof(H58B)=
 Sof(H58C)=FVAR(1)
 Sof(H25A)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=1-FVAR(2)
 Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(2)
 Sof(H59A)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=Sof(H63A)=Sof(H63B)=
 Sof(H63C)=1-FVAR(3)
 Sof(H59)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=
 Sof(H61C)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C25(H25A), C42(H42), C45(H45),
 C54(H54), C54(H54A), C59(H59), C59(H59A)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C50(H50), C51(H51),
  C52(H52), C64(H64)
7.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(H24C,H24A,H24B), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C66(H66A,H66B,H66C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.64110(14) 0.55015(9) 0.23402(9) 0.0507(4) Uani 1 1 d . . . . .
O2 O 0.72168(13) 0.68437(10) 0.15410(9) 0.0494(4) Uani 1 1 d . . . . .
N1 N 0.74226(12) 0.79559(9) 0.25910(10) 0.0336(3) Uani 1 1 d . . . . .
N2 N 0.60747(12) 0.75653(9) 0.36750(10) 0.0333(3) Uani 1 1 d . . . . .
C1 C 0.66258(14) 0.73123(11) 0.30389(11) 0.0319(3) Uani 1 1 d . . . . .
C2 C 0.73333(16) 0.85901(12) 0.29533(12) 0.0369(4) Uani 1 1 d . . . . .
H2 H 0.778188 0.910115 0.276208 0.044 Uiso 1 1 calc R U . . .
C3 C 0.65054(16) 0.83501(12) 0.36162(13) 0.0379(4) Uani 1 1 d . . . . .
H3 H 0.625770 0.865926 0.397972 0.045 Uiso 1 1 calc R U . . .
C4 C 0.84063(15) 0.79077(12) 0.20137(12) 0.0341(4) Uani 1 1 d . . . . .
C5 C 0.93263(16) 0.72533(12) 0.24132(13) 0.0393(4) Uani 1 1 d . . . . .
C6 C 1.02841(18) 0.72391(15) 0.18507(17) 0.0516(5) Uani 1 1 d . . . . .
H6 H 1.092336 0.679713 0.209893 0.062 Uiso 1 1 calc R U . . .
C7 C 1.0318(2) 0.78602(18) 0.09348(17) 0.0576(6) Uani 1 1 d . . . . .
H7 H 1.097569 0.783626 0.055876 0.069 Uiso 1 1 calc R U . . .
C8 C 0.9408(2) 0.85116(17) 0.05640(14) 0.0537(5) Uani 1 1 d . . . . .
H8 H 0.945057 0.893825 -0.006522 0.064 Uiso 1 1 calc R U . . .
C9 C 0.84239(18) 0.85587(13) 0.10938(12) 0.0425(4) Uani 1 1 d . . . . .
C10 C 0.93198(18) 0.65880(13) 0.34218(15) 0.0463(4) Uani 1 1 d . . . . .
H10 H 0.855822 0.670244 0.370034 0.056 Uiso 1 1 calc R U . . .
C11 C 1.0236(2) 0.67770(17) 0.38805(17) 0.0620(6) Uani 1 1 d . . . . .
H11A H 1.099532 0.665836 0.362866 0.093 Uiso 1 1 calc R U . . .
H11B H 1.018178 0.636291 0.453591 0.093 Uiso 1 1 calc R U . . .
H11C H 1.011997 0.743093 0.377123 0.093 Uiso 1 1 calc R U . . .
C12 C 0.9455(3) 0.55669(16) 0.3595(2) 0.0770(8) Uani 1 1 d . . . . .
H12A H 0.886805 0.546741 0.328398 0.115 Uiso 1 1 calc R U . . .
H12B H 0.936854 0.515588 0.424958 0.115 Uiso 1 1 calc R U . . .
H12C H 1.021575 0.542292 0.336265 0.115 Uiso 1 1 calc R U . . .
C13 C 0.7435(2) 0.92849(15) 0.06782(14) 0.0539(5) Uani 1 1 d . . . . .
H13 H 0.686138 0.925192 0.117955 0.065 Uiso 1 1 calc R U . . .
C14 C 0.6843(3) 0.91059(19) 0.0006(2) 0.0829(10) Uani 1 1 d . . . . .
H14A H 0.625347 0.962056 -0.028863 0.124 Uiso 1 1 calc R U . . .
H14B H 0.648737 0.851566 0.033277 0.124 Uiso 1 1 calc R U . . .
H14C H 0.740939 0.906689 -0.045564 0.124 Uiso 1 1 calc R U . . .
C15 C 0.7831(3) 1.02739(16) 0.01981(17) 0.0665(7) Uani 1 1 d . . . . .
H15A H 0.835562 1.033535 -0.032234 0.100 Uiso 1 1 calc R U . . .
H15B H 0.822558 1.038297 0.062413 0.100 Uiso 1 1 calc R U . . .
H15C H 0.716514 1.073538 -0.001411 0.100 Uiso 1 1 calc R U . . .
C16 C 0.50489(15) 0.71957(11) 0.42026(12) 0.0328(3) Uani 1 1 d . . . . .
C17 C 0.40014(16) 0.76054(13) 0.38126(12) 0.0371(4) Uani 1 1 d . . . . .
C18 C 0.30108(16) 0.72753(14) 0.43466(13) 0.0421(4) Uani 1 1 d . . . . .
H18 H 0.228362 0.755065 0.410772 0.051 Uiso 1 1 calc R U . . .
C19 C 0.30730(17) 0.65506(14) 0.52214(13) 0.0420(4) Uani 1 1 d . . . . .
H19 H 0.238857 0.632840 0.557256 0.050 Uiso 1 1 calc R U . . .
C20 C 0.41179(17) 0.61480(12) 0.55884(12) 0.0389(4) Uani 1 1 d . . . . .
H20 H 0.414552 0.564946 0.618864 0.047 Uiso 1 1 calc R U . . .
C21 C 0.51346(16) 0.64647(12) 0.50880(12) 0.0361(4) Uani 1 1 d . . . . .
C22 C 0.39171(18) 0.83884(15) 0.28477(13) 0.0464(4) Uani 1 1 d . . . . .
H22 H 0.471061 0.849051 0.256322 0.056 Uiso 1 1 calc R U . . .
C23 C 0.3374(2) 0.93023(16) 0.28450(16) 0.0560(5) Uani 1 1 d . . . . .
H23A H 0.260091 0.921384 0.313532 0.084 Uiso 1 1 calc R U . . .
H23B H 0.333280 0.979722 0.221705 0.084 Uiso 1 1 calc R U . . .
H23C H 0.384059 0.948145 0.318100 0.084 Uiso 1 1 calc R U . . .
C24 C 0.3249(3) 0.8123(2) 0.22827(17) 0.0766(8) Uani 1 1 d . . . . .
H24C H 0.363347 0.755623 0.226333 0.115 Uiso 1 1 calc R U . . .
H24A H 0.321070 0.863634 0.166357 0.115 Uiso 1 1 calc R U . . .
H24B H 0.247170 0.800472 0.255768 0.115 Uiso 1 1 calc R U . . .
C25 C 0.62769(18) 0.60447(14) 0.55101(15) 0.0503(5) Uani 1 1 d D U . . .
H25 H 0.685484 0.646886 0.509080 0.060 Uiso 0.337(15) 1 calc R U P A 1
H25A H 0.688378 0.621866 0.500488 0.060 Uiso 0.663(15) 1 calc R U P A 2
C26 C 0.6679(13) 0.5137(9) 0.5616(12) 0.072(3) Uani 0.337(15) 1 d D U P A 1
H26A H 0.735102 0.490164 0.598440 0.108 Uiso 0.337(15) 1 calc R U P A 1
H26B H 0.689006 0.516541 0.501696 0.108 Uiso 0.337(15) 1 calc R U P A 1
H26C H 0.607505 0.471566 0.591857 0.108 Uiso 0.337(15) 1 calc R U P A 1
C27 C 0.6247(11) 0.6116(9) 0.6432(7) 0.056(2) Uani 0.337(15) 1 d D U P A 1
H27A H 0.570702 0.569707 0.687703 0.084 Uiso 0.337(15) 1 calc R U P A 1
H27B H 0.600390 0.676153 0.632007 0.084 Uiso 0.337(15) 1 calc R U P A 1
H27C H 0.701328 0.593237 0.667021 0.084 Uiso 0.337(15) 1 calc R U P A 1
C28 C 0.6322(5) 0.4947(3) 0.6015(4) 0.0498(12) Uani 0.663(15) 1 d D U P A 2
H28A H 0.611045 0.472043 0.560360 0.075 Uiso 0.663(15) 1 calc R U P A 2
H28B H 0.578503 0.475278 0.654964 0.075 Uiso 0.663(15) 1 calc R U P A 2
H28C H 0.709939 0.468296 0.620799 0.075 Uiso 0.663(15) 1 calc R U P A 2
C29 C 0.6542(8) 0.6409(5) 0.6126(7) 0.091(2) Uani 0.663(15) 1 d D U P A 2
H29A H 0.592957 0.629109 0.660449 0.136 Uiso 0.663(15) 1 calc R U P A 2
H29B H 0.660375 0.708457 0.578149 0.136 Uiso 0.663(15) 1 calc R U P A 2
H29C H 0.726886 0.609425 0.640267 0.136 Uiso 0.663(15) 1 calc R U P A 2
C30 C 0.63588(16) 0.65389(12) 0.29709(12) 0.0368(4) Uani 1 1 d . . . . .
H30 H 0.589433 0.613992 0.346878 0.044 Uiso 1 1 calc R U . . .
C31 C 0.66520(16) 0.62361(12) 0.22955(12) 0.0367(4) Uani 1 1 d . . . . .
C32 C 0.7593(2) 0.65298(17) 0.08762(15) 0.0574(6) Uani 1 1 d . . . . .
H32A H 0.803684 0.699885 0.038187 0.086 Uiso 1 1 calc R U . . .
H32B H 0.692697 0.643860 0.063271 0.086 Uiso 1 1 calc R U . . .
H32C H 0.807314 0.593576 0.115643 0.086 Uiso 1 1 calc R U . . .
O3 O 0.99836(12) 0.09623(9) 0.26728(10) 0.0457(3) Uani 1 1 d . . . . .
O4 O 0.93487(11) 0.03322(9) 0.18676(9) 0.0424(3) Uani 1 1 d . . . . .
N3 N 0.72693(14) 0.31956(11) 0.13815(11) 0.0415(4) Uani 1 1 d . . . . .
N4 N 0.81554(13) 0.26271(9) 0.26399(10) 0.0341(3) Uani 1 1 d . . . . .
C33 C 0.79975(15) 0.24549(12) 0.19271(11) 0.0339(4) Uani 1 1 d . . . . .
C34 C 0.75277(17) 0.34754(12) 0.25157(13) 0.0423(4) Uani 1 1 d . . . . .
H34 H 0.749366 0.375429 0.291154 0.051 Uiso 1 1 calc R U . . .
C35 C 0.69907(18) 0.38195(13) 0.17497(14) 0.0467(5) Uani 1 1 d . . . . .
H35 H 0.650555 0.438689 0.149855 0.056 Uiso 1 1 calc R U . . .
C36 C 0.85089(16) 0.19520(11) 0.35389(11) 0.0333(4) Uani 1 1 d . . . . .
C37 C 0.95692(16) 0.19828(12) 0.38061(12) 0.0368(4) Uani 1 1 d . . . . .
C38 C 0.98419(18) 0.13743(14) 0.46994(13) 0.0440(4) Uani 1 1 d . . . . .
H38 H 1.054915 0.139895 0.490632 0.053 Uiso 1 1 calc R U . . .
C39 C 0.91006(19) 0.07368(13) 0.52877(13) 0.0462(5) Uani 1 1 d . . . . .
H39 H 0.930644 0.031623 0.588960 0.055 Uiso 1 1 calc R U . . .
C40 C 0.80633(18) 0.07124(12) 0.50000(13) 0.0431(4) Uani 1 1 d . . . . .
H40 H 0.756291 0.026638 0.540790 0.052 Uiso 1 1 calc R U . . .
C41 C 0.77265(16) 0.13261(11) 0.41238(12) 0.0372(4) Uani 1 1 d . . . . .
C42 C 1.04125(17) 0.26586(14) 0.31594(14) 0.0439(4) Uani 1 1 d . . . . .
H42 H 1.016121 0.290043 0.252812 0.053 Uiso 1 1 calc R U . . .
C43 C 1.0388(2) 0.34921(16) 0.33554(19) 0.0650(6) Uani 1 1 d . . . . .
H43A H 0.961267 0.381246 0.328809 0.098 Uiso 1 1 calc R U . . .
H43B H 1.092402 0.392751 0.292655 0.098 Uiso 1 1 calc R U . . .
H43C H 1.061053 0.327255 0.397763 0.098 Uiso 1 1 calc R U . . .
C44 C 1.16278(19) 0.21788(16) 0.31951(17) 0.0553(5) Uani 1 1 d . . . . .
H44A H 1.190936 0.195955 0.380025 0.083 Uiso 1 1 calc R U . . .
H44B H 1.213115 0.262547 0.273770 0.083 Uiso 1 1 calc R U . . .
H44C H 1.162090 0.164407 0.307032 0.083 Uiso 1 1 calc R U . . .
C45 C 0.65615(17) 0.12955(13) 0.38483(13) 0.0414(4) Uani 1 1 d . . . . .
H45 H 0.643711 0.184032 0.323717 0.050 Uiso 1 1 calc R U . . .
C46 C 0.56018(19) 0.13854(16) 0.45051(16) 0.0531(5) Uani 1 1 d . . . . .
H46A H 0.569035 0.084929 0.510725 0.080 Uiso 1 1 calc R U . . .
H46B H 0.486090 0.139865 0.428347 0.080 Uiso 1 1 calc R U . . .
H46C H 0.563738 0.196588 0.454659 0.080 Uiso 1 1 calc R U . . .
C47 C 0.6516(2) 0.04011(15) 0.37588(16) 0.0534(5) Uani 1 1 d . . . . .
H47A H 0.710998 0.037326 0.330889 0.080 Uiso 1 1 calc R U . . .
H47B H 0.576246 0.040320 0.356218 0.080 Uiso 1 1 calc R U . . .
H47C H 0.664536 -0.014579 0.434800 0.080 Uiso 1 1 calc R U . . .
C48 C 0.68970(18) 0.33380(15) 0.05260(14) 0.0476(5) Uani 1 1 d . . . . .
C49 C 0.60484(19) 0.28078(19) 0.05305(16) 0.0593(6) Uani 1 1 d . . . . .
C50 C 0.5688(2) 0.2983(3) -0.03126(19) 0.0768(8) Uani 1 1 d . . . . .
H50 H 0.512064 0.263157 -0.033540 0.092 Uiso 1 1 calc R U . . .
C51 C 0.6141(3) 0.3655(2) -0.11065(19) 0.0805(8) Uani 1 1 d . . . . .
H51 H 0.587112 0.377216 -0.167081 0.097 Uiso 1 1 calc R U . . .
C52 C 0.6976(3) 0.4157(2) -0.10939(17) 0.0721(7) Uani 1 1 d . . . . .
H52 H 0.728418 0.461281 -0.165326 0.086 Uiso 1 1 calc R U . . .
C53 C 0.7393(2) 0.40181(16) -0.02756(15) 0.0561(5) Uani 1 1 d . . . . .
C54 C 0.5524(2) 0.2076(2) 0.14133(18) 0.0683(7) Uani 1 1 d D U . . .
H54 H 0.599321 0.198189 0.191934 0.082 Uiso 0.570(14) 1 calc R U P B 1
H54A H 0.613361 0.174446 0.185814 0.082 Uiso 0.430(14) 1 calc R U P B 2
C55 C 0.4617(8) 0.2714(10) 0.1773(8) 0.103(3) Uani 0.430(14) 1 d D U P B 2
H55A H 0.401512 0.303802 0.134106 0.154 Uiso 0.430(14) 1 calc R U P B 2
H55B H 0.502340 0.317695 0.182342 0.154 Uiso 0.430(14) 1 calc R U P B 2
H55C H 0.427203 0.230869 0.237012 0.154 Uiso 0.430(14) 1 calc R U P B 2
C56 C 0.4302(6) 0.2328(7) 0.1645(7) 0.101(3) Uani 0.570(14) 1 d D U P B 1
H56A H 0.380138 0.230092 0.122663 0.151 Uiso 0.570(14) 1 calc R U P B 1
H56B H 0.422228 0.296280 0.158825 0.151 Uiso 0.570(14) 1 calc R U P B 1
H56C H 0.408642 0.188396 0.226982 0.151 Uiso 0.570(14) 1 calc R U P B 1
C57 C 0.4960(14) 0.1411(11) 0.1328(8) 0.112(4) Uani 0.430(14) 1 d D U P B 2
H57A H 0.547764 0.111363 0.101357 0.168 Uiso 0.430(14) 1 calc R U P B 2
H57B H 0.428012 0.172155 0.097681 0.168 Uiso 0.430(14) 1 calc R U P B 2
H57C H 0.472774 0.093286 0.193281 0.168 Uiso 0.430(14) 1 calc R U P B 2
C58 C 0.5552(8) 0.1075(4) 0.1406(4) 0.0693(18) Uani 0.570(14) 1 d D U P B 1
H58A H 0.524404 0.061609 0.199392 0.104 Uiso 0.570(14) 1 calc R U P B 1
H58B H 0.634360 0.085875 0.129833 0.104 Uiso 0.570(14) 1 calc R U P B 1
H58C H 0.508675 0.114419 0.092201 0.104 Uiso 0.570(14) 1 calc R U P B 1
C59 C 0.8328(2) 0.45694(15) -0.02732(16) 0.0623(6) Uani 1 1 d D U . . .
H59 H 0.847795 0.439465 0.036897 0.075 Uiso 0.797(18) 1 calc R U P C 1
H59A H 0.824255 0.444714 0.037674 0.075 Uiso 0.203(18) 1 calc R U P C 2
C60 C 0.7901(9) 0.5617(3) -0.0762(5) 0.081(2) Uani 0.797(18) 1 d D U P C 1
H60A H 0.785749 0.581140 -0.141106 0.121 Uiso 0.797(18) 1 calc R U P C 1
H60B H 0.843430 0.598439 -0.068166 0.121 Uiso 0.797(18) 1 calc R U P C 1
H60C H 0.714065 0.572046 -0.050320 0.121 Uiso 0.797(18) 1 calc R U P C 1
C61 C 0.9429(4) 0.4371(5) -0.0752(6) 0.0740(15) Uani 0.797(18) 1 d D U P C 1
H61A H 0.970523 0.370754 -0.042458 0.111 Uiso 0.797(18) 1 calc R U P C 1
H61B H 1.001049 0.475635 -0.076464 0.111 Uiso 0.797(18) 1 calc R U P C 1
H61C H 0.927905 0.452237 -0.137607 0.111 Uiso 0.797(18) 1 calc R U P C 1
C62 C 0.840(3) 0.5641(9) -0.074(2) 0.083(6) Uani 0.203(18) 1 d D U P C 2
H62A H 0.844272 0.587899 -0.140184 0.125 Uiso 0.203(18) 1 calc R U P C 2
H62B H 0.909051 0.577646 -0.055961 0.125 Uiso 0.203(18) 1 calc R U P C 2
H62C H 0.772352 0.594583 -0.055623 0.125 Uiso 0.203(18) 1 calc R U P C 2
C63 C 0.9523(13) 0.4057(16) -0.028(2) 0.079(4) Uani 0.203(18) 1 d D U P C 2
H63A H 0.963509 0.351600 0.031804 0.118 Uiso 0.203(18) 1 calc R U P C 2
H63B H 1.010777 0.448490 -0.040851 0.118 Uiso 0.203(18) 1 calc R U P C 2
H63C H 0.958559 0.384342 -0.074619 0.118 Uiso 0.203(18) 1 calc R U P C 2
C64 C 0.84031(16) 0.17167(12) 0.17379(12) 0.0361(4) Uani 1 1 d . . . . .
H64 H 0.803843 0.167673 0.127723 0.043 Uiso 1 1 calc R U . . .
C65 C 0.92971(15) 0.10178(12) 0.21525(12) 0.0336(4) Uani 1 1 d . . . . .
C66 C 1.02876(17) -0.03731(13) 0.21745(14) 0.0444(4) Uani 1 1 d . . . . .
H66A H 1.027880 -0.080042 0.190837 0.067 Uiso 1 1 calc R U . . .
H66B H 1.022087 -0.072501 0.283873 0.067 Uiso 1 1 calc R U . . .
H66C H 1.100759 -0.007800 0.198708 0.067 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
O1 C31 1.226(2) . ?
O2 C31 1.354(2) . ?
O2 C32 1.424(2) . ?
N1 C1 1.384(2) . ?
N1 C2 1.399(2) . ?
N1 C4 1.440(2) . ?
N2 C1 1.374(2) . ?
N2 C3 1.389(2) . ?
N2 C16 1.438(2) . ?
C1 C30 1.387(2) . ?
C2 C3 1.337(3) . ?
C4 C5 1.394(3) . ?
C4 C9 1.399(2) . ?
C5 C6 1.390(3) . ?
C5 C10 1.516(3) . ?
C6 C7 1.382(3) . ?
C7 C8 1.373(4) . ?
C8 C9 1.394(3) . ?
C9 C13 1.510(3) . ?
C10 C11 1.528(3) . ?
C10 C12 1.529(3) . ?
C13 C14 1.533(3) . ?
C13 C15 1.534(3) . ?
C16 C17 1.396(3) . ?
C16 C21 1.402(2) . ?
C17 C18 1.393(3) . ?
C17 C22 1.519(3) . ?
C18 C19 1.385(3) . ?
C19 C20 1.379(3) . ?
C20 C21 1.395(3) . ?
C21 C25 1.515(3) . ?
C22 C23 1.529(3) . ?
C22 C24 1.523(3) . ?
C25 C26 1.417(9) . ?
C25 C27 1.586(8) . ?
C25 C28 1.571(4) . ?
C25 C29 1.475(7) . ?
C30 C31 1.414(2) . ?
O3 C65 1.215(2) . ?
O4 C65 1.386(2) . ?
O4 C66 1.428(2) . ?
N3 C33 1.374(2) . ?
N3 C35 1.393(2) . ?
N3 C48 1.441(2) . ?
N4 C33 1.373(2) . ?
N4 C34 1.405(2) . ?
N4 C36 1.451(2) . ?
C33 C64 1.384(2) . ?
C34 C35 1.327(3) . ?
C36 C37 1.388(3) . ?
C36 C41 1.402(2) . ?
C37 C38 1.395(3) . ?
C37 C42 1.520(3) . ?
C38 C39 1.380(3) . ?
C39 C40 1.375(3) . ?
C40 C41 1.396(3) . ?
C41 C45 1.511(3) . ?
C42 C43 1.524(3) . ?
C42 C44 1.531(3) . ?
C45 C46 1.525(3) . ?
C45 C47 1.530(2) . ?
C48 C49 1.401(4) . ?
C48 C53 1.404(3) . ?
C49 C50 1.399(3) . ?
C49 C54 1.525(4) . ?
C50 C51 1.371(4) . ?
C51 C52 1.368(5) . ?
C52 C53 1.406(3) . ?
C53 C59 1.511(4) . ?
C54 C55 1.645(10) . ?
C54 C56 1.503(7) . ?
C54 C57 1.407(9) . ?
C54 C58 1.622(6) . ?
C59 C60 1.540(5) . ?
C59 C61 1.524(5) . ?
C59 C62 1.548(13) . ?
C59 C63 1.539(13) . ?
C64 C65 1.410(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C31 O2 C32 115.98(15) . . ?
C1 N1 C2 109.45(14) . . ?
C1 N1 C4 128.73(14) . . ?
C2 N1 C4 120.05(13) . . ?
C1 N2 C3 110.65(14) . . ?
C1 N2 C16 124.73(13) . . ?
C3 N2 C16 123.53(14) . . ?
N1 C1 C30 133.75(16) . . ?
N2 C1 N1 104.63(13) . . ?
N2 C1 C30 121.59(15) . . ?
C3 C2 N1 107.96(14) . . ?
C2 C3 N2 107.31(15) . . ?
C5 C4 N1 118.15(16) . . ?
C5 C4 C9 123.18(17) . . ?
C9 C4 N1 118.52(17) . . ?
C4 C5 C10 122.57(17) . . ?
C6 C5 C4 117.34(19) . . ?
C6 C5 C10 120.08(19) . . ?
C7 C6 C5 120.8(2) . . ?
C8 C7 C6 120.5(2) . . ?
C7 C8 C9 121.2(2) . . ?
C4 C9 C13 122.53(18) . . ?
C8 C9 C4 116.8(2) . . ?
C8 C9 C13 120.63(19) . . ?
C5 C10 C11 111.32(17) . . ?
C5 C10 C12 111.31(19) . . ?
C11 C10 C12 111.10(19) . . ?
C9 C13 C14 112.0(2) . . ?
C9 C13 C15 111.03(19) . . ?
C14 C13 C15 109.49(18) . . ?
C17 C16 N2 117.92(15) . . ?
C17 C16 C21 122.80(16) . . ?
C21 C16 N2 119.25(16) . . ?
C16 C17 C22 122.45(16) . . ?
C18 C17 C16 117.46(17) . . ?
C18 C17 C22 120.09(17) . . ?
C19 C18 C17 120.81(18) . . ?
C20 C19 C18 120.71(17) . . ?
C19 C20 C21 120.72(17) . . ?
C16 C21 C25 122.15(16) . . ?
C20 C21 C16 117.47(17) . . ?
C20 C21 C25 120.35(17) . . ?
C17 C22 C23 110.91(17) . . ?
C17 C22 C24 111.04(18) . . ?
C24 C22 C23 110.6(2) . . ?
C21 C25 C27 108.3(5) . . ?
C21 C25 C28 110.4(2) . . ?
C26 C25 C21 117.3(5) . . ?
C26 C25 C27 112.4(6) . . ?
C29 C25 C21 112.8(4) . . ?
C29 C25 C28 110.7(4) . . ?
C1 C30 C31 131.72(16) . . ?
O1 C31 O2 119.85(16) . . ?
O1 C31 C30 125.36(16) . . ?
O2 C31 C30 114.76(15) . . ?
C65 O4 C66 115.48(14) . . ?
C33 N3 C35 110.13(15) . . ?
C33 N3 C48 125.17(15) . . ?
C35 N3 C48 124.61(16) . . ?
C33 N4 C34 109.10(15) . . ?
C33 N4 C36 127.45(13) . . ?
C34 N4 C36 119.70(14) . . ?
N3 C33 C64 122.94(16) . . ?
N4 C33 N3 105.19(14) . . ?
N4 C33 C64 131.84(16) . . ?
C35 C34 N4 108.16(16) . . ?
C34 C35 N3 107.42(16) . . ?
C37 C36 N4 119.39(15) . . ?
C37 C36 C41 122.58(16) . . ?
C41 C36 N4 117.92(16) . . ?
C36 C37 C38 117.82(17) . . ?
C36 C37 C42 121.87(16) . . ?
C38 C37 C42 120.31(17) . . ?
C39 C38 C37 121.06(19) . . ?
C40 C39 C38 119.81(18) . . ?
C39 C40 C41 121.70(18) . . ?
C36 C41 C45 123.20(16) . . ?
C40 C41 C36 116.98(18) . . ?
C40 C41 C45 119.82(16) . . ?
C37 C42 C43 110.33(17) . . ?
C37 C42 C44 112.09(17) . . ?
C43 C42 C44 111.00(18) . . ?
C41 C45 C46 112.11(16) . . ?
C41 C45 C47 110.70(16) . . ?
C46 C45 C47 110.63(16) . . ?
C49 C48 N3 118.87(19) . . ?
C49 C48 C53 123.1(2) . . ?
C53 C48 N3 118.0(2) . . ?
C48 C49 C54 121.8(2) . . ?
C50 C49 C48 117.2(2) . . ?
C50 C49 C54 121.0(2) . . ?
C51 C50 C49 121.1(3) . . ?
C52 C51 C50 120.7(2) . . ?
C51 C52 C53 121.8(3) . . ?
C48 C53 C52 116.2(2) . . ?
C48 C53 C59 122.6(2) . . ?
C52 C53 C59 121.2(2) . . ?
C49 C54 C55 102.9(5) . . ?
C49 C54 C58 111.9(3) . . ?
C56 C54 C49 115.2(4) . . ?
C56 C54 C58 106.3(5) . . ?
C57 C54 C49 115.5(5) . . ?
C57 C54 C55 110.6(6) . . ?
C53 C59 C60 107.8(4) . . ?
C53 C59 C61 111.1(2) . . ?
C53 C59 C62 129.8(13) . . ?
C53 C59 C63 111.7(7) . . ?
C61 C59 C60 110.2(3) . . ?
C63 C59 C62 110.1(11) . . ?
C33 C64 C65 127.25(16) . . ?
O3 C65 O4 120.04(15) . . ?
O3 C65 C64 129.90(16) . . ?
O4 C65 C64 110.04(14) . . ?

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 C30 C31 -14.7(4) . . . . ?
N1 C2 C3 N2 0.2(2) . . . . ?
N1 C4 C5 C6 -177.80(15) . . . . ?
N1 C4 C5 C10 0.9(2) . . . . ?
N1 C4 C9 C8 177.69(15) . . . . ?
N1 C4 C9 C13 -2.3(2) . . . . ?
N2 C1 C30 C31 167.64(19) . . . . ?
N2 C16 C17 C18 -176.70(15) . . . . ?
N2 C16 C17 C22 2.7(2) . . . . ?
N2 C16 C21 C20 177.82(14) . . . . ?
N2 C16 C21 C25 -0.3(2) . . . . ?
C1 N1 C2 C3 0.3(2) . . . . ?
C1 N1 C4 C5 -69.6(2) . . . . ?
C1 N1 C4 C9 114.59(19) . . . . ?
C1 N2 C3 C2 -0.6(2) . . . . ?
C1 N2 C16 C17 -84.1(2) . . . . ?
C1 N2 C16 C21 97.7(2) . . . . ?
C1 C30 C31 O1 175.6(2) . . . . ?
C1 C30 C31 O2 -6.3(3) . . . . ?
C2 N1 C1 N2 -0.65(19) . . . . ?
C2 N1 C1 C30 -178.60(19) . . . . ?
C2 N1 C4 C5 93.52(19) . . . . ?
C2 N1 C4 C9 -82.3(2) . . . . ?
C3 N2 C1 N1 0.77(19) . . . . ?
C3 N2 C1 C30 179.03(17) . . . . ?
C3 N2 C16 C17 82.8(2) . . . . ?
C3 N2 C16 C21 -95.4(2) . . . . ?
C4 N1 C1 N2 163.90(16) . . . . ?
C4 N1 C1 C30 -14.0(3) . . . . ?
C4 N1 C2 C3 -165.81(16) . . . . ?
C4 C5 C6 C7 0.7(3) . . . . ?
C4 C5 C10 C11 -115.6(2) . . . . ?
C4 C5 C10 C12 119.8(2) . . . . ?
C4 C9 C13 C14 -112.2(2) . . . . ?
C4 C9 C13 C15 125.1(2) . . . . ?
C5 C4 C9 C8 2.1(3) . . . . ?
C5 C4 C9 C13 -177.85(17) . . . . ?
C5 C6 C7 C8 0.7(3) . . . . ?
C6 C5 C10 C11 63.0(2) . . . . ?
C6 C5 C10 C12 -61.5(2) . . . . ?
C6 C7 C8 C9 -0.8(3) . . . . ?
C7 C8 C9 C4 -0.6(3) . . . . ?
C7 C8 C9 C13 179.41(19) . . . . ?
C8 C9 C13 C14 67.8(3) . . . . ?
C8 C9 C13 C15 -54.9(3) . . . . ?
C9 C4 C5 C6 -2.2(2) . . . . ?
C9 C4 C5 C10 176.49(16) . . . . ?
C10 C5 C6 C7 -178.00(18) . . . . ?
C16 N2 C1 N1 169.17(15) . . . . ?
C16 N2 C1 C30 -12.6(3) . . . . ?
C16 N2 C3 C2 -169.17(16) . . . . ?
C16 C17 C18 C19 -1.7(3) . . . . ?
C16 C17 C22 C23 -113.3(2) . . . . ?
C16 C17 C22 C24 123.2(2) . . . . ?
C16 C21 C25 C26 -107.4(10) . . . . ?
C16 C21 C25 C27 124.1(5) . . . . ?
C16 C21 C25 C28 -135.7(3) . . . . ?
C16 C21 C25 C29 99.9(5) . . . . ?
C17 C16 C21 C20 -0.3(2) . . . . ?
C17 C16 C21 C25 -178.36(17) . . . . ?
C17 C18 C19 C20 0.9(3) . . . . ?
C18 C17 C22 C23 66.1(2) . . . . ?
C18 C17 C22 C24 -57.3(3) . . . . ?
C18 C19 C20 C21 0.3(3) . . . . ?
C19 C20 C21 C16 -0.6(2) . . . . ?
C19 C20 C21 C25 177.52(17) . . . . ?
C20 C21 C25 C26 74.6(10) . . . . ?
C20 C21 C25 C27 -53.9(6) . . . . ?
C20 C21 C25 C28 46.3(4) . . . . ?
C20 C21 C25 C29 -78.1(5) . . . . ?
C21 C16 C17 C18 1.4(2) . . . . ?
C21 C16 C17 C22 -179.12(17) . . . . ?
C22 C17 C18 C19 178.81(17) . . . . ?
C32 O2 C31 O1 -6.0(3) . . . . ?
C32 O2 C31 C30 175.81(18) . . . . ?
N3 C33 C64 C65 167.78(17) . . . . ?
N3 C48 C49 C50 178.4(2) . . . . ?
N3 C48 C49 C54 -1.0(3) . . . . ?
N3 C48 C53 C52 -177.86(19) . . . . ?
N3 C48 C53 C59 2.7(3) . . . . ?
N4 C33 C64 C65 -14.3(3) . . . . ?
N4 C34 C35 N3 0.1(2) . . . . ?
N4 C36 C37 C38 174.83(15) . . . . ?
N4 C36 C37 C42 -4.6(2) . . . . ?
N4 C36 C41 C40 -177.02(14) . . . . ?
N4 C36 C41 C45 2.7(2) . . . . ?
C33 N3 C35 C34 -0.4(2) . . . . ?
C33 N3 C48 C49 77.1(3) . . . . ?
C33 N3 C48 C53 -104.0(2) . . . . ?
C33 N4 C34 C35 0.2(2) . . . . ?
C33 N4 C36 C37 112.80(19) . . . . ?
C33 N4 C36 C41 -70.9(2) . . . . ?
C33 C64 C65 O3 -9.6(3) . . . . ?
C33 C64 C65 O4 171.96(17) . . . . ?
C34 N4 C33 N3 -0.46(19) . . . . ?
C34 N4 C33 C64 -178.64(19) . . . . ?
C34 N4 C36 C37 -91.5(2) . . . . ?
C34 N4 C36 C41 84.80(19) . . . . ?
C35 N3 C33 N4 0.5(2) . . . . ?
C35 N3 C33 C64 178.90(18) . . . . ?
C35 N3 C48 C49 -106.6(2) . . . . ?
C35 N3 C48 C53 72.3(3) . . . . ?
C36 N4 C33 N3 157.32(16) . . . . ?
C36 N4 C33 C64 -20.9(3) . . . . ?
C36 N4 C34 C35 -159.54(17) . . . . ?
C36 C37 C38 C39 2.5(3) . . . . ?
C36 C37 C42 C43 101.7(2) . . . . ?
C36 C37 C42 C44 -134.01(19) . . . . ?
C36 C41 C45 C46 -126.09(19) . . . . ?
C36 C41 C45 C47 109.86(19) . . . . ?
C37 C36 C41 C40 -0.9(2) . . . . ?
C37 C36 C41 C45 178.89(16) . . . . ?
C37 C38 C39 C40 -1.6(3) . . . . ?
C38 C37 C42 C43 -77.7(2) . . . . ?
C38 C37 C42 C44 46.6(2) . . . . ?
C38 C39 C40 C41 -0.7(3) . . . . ?
C39 C40 C41 C36 1.9(3) . . . . ?
C39 C40 C41 C45 -177.89(17) . . . . ?
C40 C41 C45 C46 53.7(2) . . . . ?
C40 C41 C45 C47 -70.4(2) . . . . ?
C41 C36 C37 C38 -1.3(2) . . . . ?
C41 C36 C37 C42 179.29(16) . . . . ?
C42 C37 C38 C39 -178.04(17) . . . . ?
C48 N3 C33 N4 177.21(18) . . . . ?
C48 N3 C33 C64 -4.4(3) . . . . ?
C48 N3 C35 C34 -177.09(19) . . . . ?
C48 C49 C50 C51 -0.7(4) . . . . ?
C48 C49 C54 C55 77.9(5) . . . . ?
C48 C49 C54 C56 109.5(6) . . . . ?
C48 C49 C54 C57 -161.4(9) . . . . ?
C48 C49 C54 C58 -128.9(4) . . . . ?
C48 C53 C59 C60 -121.9(4) . . . . ?
C48 C53 C59 C61 117.2(4) . . . . ?
C48 C53 C59 C62 -128.0(18) . . . . ?
C48 C53 C59 C63 87.8(15) . . . . ?
C49 C48 C53 C52 1.0(3) . . . . ?
C49 C48 C53 C59 -178.5(2) . . . . ?
C49 C50 C51 C52 1.4(5) . . . . ?
C50 C49 C54 C55 -101.4(6) . . . . ?
C50 C49 C54 C56 -69.8(7) . . . . ?
C50 C49 C54 C57 19.3(9) . . . . ?
C50 C49 C54 C58 51.8(4) . . . . ?
C50 C51 C52 C53 -0.9(5) . . . . ?
C51 C52 C53 C48 -0.3(4) . . . . ?
C51 C52 C53 C59 179.2(3) . . . . ?
C52 C53 C59 C60 58.6(4) . . . . ?
C52 C53 C59 C61 -62.2(5) . . . . ?
C52 C53 C59 C62 52.6(18) . . . . ?
C52 C53 C59 C63 -91.6(15) . . . . ?
C53 C48 C49 C50 -0.5(3) . . . . ?
C53 C48 C49 C54 -179.8(2) . . . . ?
C54 C49 C50 C51 178.6(3) . . . . ?
C66 O4 C65 O3 -4.2(2) . . . . ?
C66 O4 C65 C64 174.45(16) . . . . ?

_olex2_date_sample_data_collection 2021-05-11
_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 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.724
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.611(2) 23643 2909 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.389(2) 0 2909 nmt 0.9956 -0.0387 0.0599 0.0180 0.9942 0.0078 -0.0831
-0.0015 1.0054

_twin_special_details            
;
Component 2 rotated by 4.2587° 
around [0.02 0.84 0.54] (reciprocal) or [-0.17 0.96 0.22] (direct)
;
####################################################################### 
# 
# 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_wf446gacl3
_database_code_depnum_ccdc_archive 'CCDC 2094752'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-05-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H36 Cl3 Ga N2 O, 0.5 (C7 H7)'
_chemical_formula_sum            'C32.50 H39.50 Cl3 Ga N2 O'
_chemical_formula_weight         650.23
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32.50 H39.50 Cl3 Ga N2 O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.39335(14)
_cell_length_b                   19.4815(2)
_cell_length_c                   16.5164(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.7901(13)
_cell_angle_gamma                90
_cell_volume                     3285.08(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14839
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4990
_cell_measurement_theta_min      3.4920
_shelx_estimated_absorpt_T_max   0.900
_shelx_estimated_absorpt_T_min   0.580
_exptl_absorpt_coefficient_mu    3.593
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.109a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1354
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0928
0 1 0 0.0534
-1 -2 2 0.0496
2 1 -2 0.0444
-1 0 1 0.0348
1 0 1 0.0223
-1 0 -1 0.0125
-1 -1 -1 0.0279

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
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
-0.0000 -1.0000 0.0000 -0.0247 0.0022 0.0750
0.0000 1.0000 -0.0000 0.0247 -0.0022 -0.0750
-1.0000 -2.0000 2.0000 -0.0370 0.2235 0.1476
2.0000 1.0000 -2.0000 0.1296 -0.3069 -0.0314
-1.0000 -0.0000 1.0000 -0.0524 0.1523 -0.0218
1.0000 -0.0000 1.0000 0.1821 -0.0189 0.0605
-1.0000 0.0000 -1.0000 -0.1821 0.0189 -0.0605
-1.0000 -1.0000 -1.0000 -0.2068 0.0212 0.0145

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28001
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.609
_diffrn_reflns_theta_min         3.545
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00  -9.00   1.00    6.00    --  -43.13 -24.00 -86.00  111
  2  ω    -25.00  35.00   1.00    6.00    --  -43.13  24.00  77.00   60
  3  ω     70.00 121.00   1.00    6.00    --   43.13  24.00  77.00   51
  4  ω     27.00  64.00   1.00    6.00    --   43.13 -24.00 -86.00   37
  5  ω     60.00  86.00   1.00   24.00    --  103.80 -24.00 -86.00   26
  6  ω     70.00 164.00   1.00   24.00    --  103.80  24.00  77.00   94
  7  ω    -61.00 -18.00   1.00    6.00    --  -43.13 125.00 150.00   43
  8  ω     74.00  99.00   1.00    6.00    --   43.13-125.00   0.00   25
  9  ω     28.00  82.00   1.00    6.00    --   43.13 -99.00 -30.00   54
 10  ω     30.00  98.00   1.00    6.00    --   43.13-125.00-150.00   68
 11  ω     76.00 108.00   1.00   24.00    --  103.80-111.00 120.00   32
 12  ω    132.00 163.00   1.00   24.00    --  103.80  77.00 -90.00   31
 13  ω    103.00 177.00   1.00   24.00    --  103.80  77.00 -30.00   74
 14  ω    103.00 176.00   1.00   24.00    --  103.80  77.00 120.00   73
 15  ω    111.00 177.00   1.00   24.00    --  103.80 111.00   0.00   66
 16  ω     36.00  62.00   1.00   24.00    --  103.80-111.00 120.00   26
 17  ω     52.00  78.00   1.00   24.00    --  103.80-111.00-150.00   26
 18  ω    103.00 177.00   1.00   24.00    --  103.80  77.00  90.00   74
 19  ω     31.00  58.00   1.00   24.00    --  103.80-111.00 -60.00   27
 20  ω     74.00 100.00   1.00   24.00    --  103.80-111.00 -60.00   26
 21  ω     53.00 106.00   1.00   24.00    --  103.80 -94.00   0.00   53
 22  ω     44.00 133.00   1.00   24.00    --  103.80 -61.00   0.00   89
 23  ω     37.00 107.00   1.00   24.00    --  103.80 -94.00 -60.00   70
 24  ω     26.00 108.00   1.00   24.00    --  103.80-103.00-167.26   82
 25  ω     44.00  69.00   1.00   24.00    --  103.80 -94.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1172488000
_diffrn_orient_matrix_UB_12      0.0247032000
_diffrn_orient_matrix_UB_13      0.0648253000
_diffrn_orient_matrix_UB_21      -0.0856212000
_diffrn_orient_matrix_UB_22      -0.0022340000
_diffrn_orient_matrix_UB_23      0.0666966000
_diffrn_orient_matrix_UB_31      0.0411694000
_diffrn_orient_matrix_UB_32      -0.0750399000
_diffrn_orient_matrix_UB_33      0.0193594000
_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                5515
_reflns_number_total             6441
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6441
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.041
_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)+(0.0474P)²+1.3924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0877
_refine_special_details          ?
_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. Restrained distances
 Ga1-Cl1A \\sim Ga1-Cl1B \\sim Ga1-Cl3A \\sim Ga1-Cl3B \\sim Ga1-Cl2B \\sim
Ga1-Cl2A
 with sigma of 0.02
 Cl1A-Cl2A \\sim Cl2A-Cl3A \\sim Cl3A-Cl1A
 with sigma of 0.02
 Cl2B-Cl1B \\sim Cl1B-Cl3B \\sim Cl3B-Cl2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32 \\sim C33 \\sim C34 \\sim C35: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(Cl1A) = Uanis(Cl1B)
Uanis(Cl3A) = Uanis(Cl3B)
4. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(1)
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C26(H26), C29(H29)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C22(H22), C23(H23), C24(H24),
 C33(H33), C34(H34)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.50709(2) 0.14910(2) 0.72099(2) 0.02788(8) Uani 1 1 d D . . . .
Cl1A Cl 0.4707(4) 0.04521(16) 0.6726(3) 0.0350(4) Uani 0.757(18) 1 d D . P A 1
Cl1B Cl 0.4566(12) 0.0481(5) 0.6829(7) 0.0350(4) Uani 0.243(18) 1 d D . P A 2
Cl2A Cl 0.3527(3) 0.17908(19) 0.7875(2) 0.0437(5) Uani 0.757(18) 1 d D . P A 1
Cl2B Cl 0.3877(19) 0.1877(6) 0.8039(9) 0.054(2) Uani 0.243(18) 1 d D . P A 2
Cl3A Cl 0.6947(4) 0.14783(14) 0.8056(3) 0.0400(5) Uani 0.757(18) 1 d D . P A 1
Cl3B Cl 0.7122(9) 0.1457(5) 0.7910(5) 0.0400(5) Uani 0.243(18) 1 d D . P A 2
O1 O 0.74454(13) 0.26766(8) 0.66819(9) 0.0370(3) Uani 1 1 d . . . . .
N1 N 0.30287(14) 0.23262(7) 0.54111(9) 0.0204(3) Uani 1 1 d . . . . .
N2 N 0.40484(14) 0.32840(7) 0.57517(9) 0.0204(3) Uani 1 1 d . . . . .
C2 C 0.41235(16) 0.25973(8) 0.58702(10) 0.0198(3) Uani 1 1 d . . . . .
C4 C 0.29149(17) 0.34448(9) 0.52031(11) 0.0237(3) Uani 1 1 d . . . . .
H4 H 0.263493 0.389025 0.501262 0.028 Uiso 1 1 calc R U . . .
C5 C 0.22820(17) 0.28500(9) 0.49896(11) 0.0242(3) Uani 1 1 d . . . . .
H5 H 0.147175 0.279834 0.461797 0.029 Uiso 1 1 calc R U . . .
C6 C 0.51770(17) 0.22366(9) 0.63845(11) 0.0229(3) Uani 1 1 d . . . . .
C7 C 0.63642(19) 0.25015(9) 0.65243(11) 0.0270(4) Uani 1 1 d . . . . .
C8 C 0.27432(17) 0.16040(8) 0.52466(11) 0.0220(3) Uani 1 1 d . . . . .
C9 C 0.34701(17) 0.12590(9) 0.47389(11) 0.0236(3) Uani 1 1 d . . . . .
C10 C 0.31472(19) 0.05716(9) 0.45644(12) 0.0292(4) Uani 1 1 d . . . . .
H10 H 0.362316 0.031517 0.422958 0.035 Uiso 1 1 calc R U . . .
C11 C 0.21457(19) 0.02598(9) 0.48718(13) 0.0318(4) Uani 1 1 d . . . . .
H11 H 0.194418 -0.020854 0.474751 0.038 Uiso 1 1 calc R U . . .
C12 C 0.14339(19) 0.06204(10) 0.53575(13) 0.0303(4) Uani 1 1 d . . . . .
H12 H 0.074595 0.039637 0.555962 0.036 Uiso 1 1 calc R U . . .
C13 C 0.17062(18) 0.13073(9) 0.55568(11) 0.0261(4) Uani 1 1 d . . . . .
C14 C 0.45275(18) 0.15993(9) 0.43604(12) 0.0269(4) Uani 1 1 d . . . . .
H14 H 0.464665 0.207788 0.458073 0.032 Uiso 1 1 calc R U . . .
C15 C 0.5838(2) 0.12244(11) 0.45986(14) 0.0351(4) Uani 1 1 d . . . . .
H15A H 0.607368 0.119156 0.520028 0.053 Uiso 1 1 calc R U . . .
H15B H 0.651846 0.147946 0.438785 0.053 Uiso 1 1 calc R U . . .
H15C H 0.576096 0.076220 0.436033 0.053 Uiso 1 1 calc R U . . .
C16 C 0.4111(2) 0.16439(14) 0.34219(14) 0.0456(5) Uani 1 1 d . . . . .
H16A H 0.401046 0.117992 0.318944 0.068 Uiso 1 1 calc R U . . .
H16B H 0.478155 0.189119 0.319201 0.068 Uiso 1 1 calc R U . . .
H16C H 0.327574 0.188918 0.328370 0.068 Uiso 1 1 calc R U . . .
C17 C 0.0861(2) 0.17038(10) 0.60520(13) 0.0324(4) Uani 1 1 d . . . . .
H17 H 0.135799 0.212006 0.628693 0.039 Uiso 1 1 calc R U . . .
C18 C -0.0406(2) 0.19414(12) 0.54922(16) 0.0425(5) Uani 1 1 d . . . . .
H18A H -0.019236 0.223470 0.505393 0.064 Uiso 1 1 calc R U . . .
H18B H -0.093722 0.220100 0.581780 0.064 Uiso 1 1 calc R U . . .
H18C H -0.090046 0.154028 0.524682 0.064 Uiso 1 1 calc R U . . .
C19 C 0.0513(3) 0.12844(14) 0.67669(16) 0.0508(6) Uani 1 1 d . . . . .
H19A H -0.009337 0.091517 0.654684 0.076 Uiso 1 1 calc R U . . .
H19B H 0.009679 0.158414 0.711913 0.076 Uiso 1 1 calc R U . . .
H19C H 0.131190 0.108581 0.709152 0.076 Uiso 1 1 calc R U . . .
C20 C 0.50758(17) 0.37645(8) 0.60845(11) 0.0224(3) Uani 1 1 d . . . . .
C21 C 0.59104(18) 0.39828(9) 0.55632(12) 0.0270(4) Uani 1 1 d . . . . .
C22 C 0.6920(2) 0.44262(10) 0.59037(14) 0.0356(4) Uani 1 1 d . . . . .
H22 H 0.750757 0.459036 0.557088 0.043 Uiso 1 1 calc R U . . .
C23 C 0.7081(2) 0.46306(10) 0.67165(15) 0.0389(5) Uani 1 1 d . . . . .
H23 H 0.778900 0.492430 0.693934 0.047 Uiso 1 1 calc R U . . .
C24 C 0.6225(2) 0.44129(10) 0.72092(13) 0.0339(4) Uani 1 1 d . . . . .
H24 H 0.634519 0.456578 0.776448 0.041 Uiso 1 1 calc R U . . .
C25 C 0.51849(19) 0.39720(9) 0.69073(11) 0.0261(4) Uani 1 1 d . . . . .
C26 C 0.5777(2) 0.37428(10) 0.46740(13) 0.0320(4) Uani 1 1 d . . . . .
H26 H 0.487249 0.355652 0.449409 0.038 Uiso 1 1 calc R U . . .
C27 C 0.5966(3) 0.43281(12) 0.40927(15) 0.0458(5) Uani 1 1 d . . . . .
H27A H 0.574424 0.416800 0.352106 0.069 Uiso 1 1 calc R U . . .
H27B H 0.688132 0.447969 0.421146 0.069 Uiso 1 1 calc R U . . .
H27C H 0.539427 0.471236 0.417249 0.069 Uiso 1 1 calc R U . . .
C28 C 0.6749(2) 0.31656(11) 0.46058(14) 0.0393(5) Uani 1 1 d . . . . .
H28A H 0.764419 0.333159 0.479830 0.059 Uiso 1 1 calc R U . . .
H28B H 0.664829 0.301931 0.402968 0.059 Uiso 1 1 calc R U . . .
H28C H 0.657723 0.277615 0.494579 0.059 Uiso 1 1 calc R U . . .
C29 C 0.4227(2) 0.37515(10) 0.74421(12) 0.0316(4) Uani 1 1 d . . . . .
H29 H 0.370870 0.335708 0.716295 0.038 Uiso 1 1 calc R U . . .
C30 C 0.3280(4) 0.43299(16) 0.7513(3) 0.0809(12) Uani 1 1 d . . . . .
H30A H 0.376165 0.472130 0.779360 0.121 Uiso 1 1 calc R U . . .
H30B H 0.262741 0.417287 0.782970 0.121 Uiso 1 1 calc R U . . .
H30C H 0.283769 0.446978 0.696044 0.121 Uiso 1 1 calc R U . . .
C31 C 0.4924(4) 0.35078(18) 0.82873(16) 0.0719(10) Uani 1 1 d . . . . .
H31A H 0.554172 0.314151 0.822068 0.108 Uiso 1 1 calc R U . . .
H31B H 0.427701 0.333253 0.859789 0.108 Uiso 1 1 calc R U . . .
H31C H 0.540039 0.389242 0.858707 0.108 Uiso 1 1 calc R U . . .
C32 C 0.0148(2) 0.44504(15) 0.5583(2) 0.0602(8) Uani 1 1 d . U . . .
C33 C 0.0246(2) 0.51405(15) 0.5832(2) 0.0586(8) Uani 1 1 d . U . . .
H33 H 0.041964 0.524541 0.640393 0.070 Uiso 1 1 calc R U . . .
C34 C 0.0095(2) 0.56714(15) 0.5266(2) 0.0592(8) Uani 1 1 d . U . . .
H34 H 0.015850 0.613156 0.545985 0.071 Uiso 1 1 calc R U . . .
C35 C 0.0240(5) 0.3822(3) 0.6296(3) 0.0478(11) Uani 0.5 1 d . U P . .
H35A H 0.039595 0.402581 0.684845 0.072 Uiso 0.5 1 calc R U P . .
H35B H 0.096168 0.351089 0.624602 0.072 Uiso 0.5 1 calc R U P . .
H35C H -0.058492 0.356469 0.620812 0.072 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 Cl1A 2.183(3) . ?
Ga1 Cl1B 2.102(10) . ?
Ga1 Cl2A 2.188(3) . ?
Ga1 Cl2B 2.148(9) . ?
Ga1 Cl3A 2.176(2) . ?
Ga1 Cl3B 2.228(8) . ?
Ga1 C6 2.0092(17) . ?
O1 C7 1.156(2) . ?
N1 C2 1.351(2) . ?
N1 C5 1.388(2) . ?
N1 C8 1.453(2) . ?
N2 C2 1.352(2) . ?
N2 C4 1.381(2) . ?
N2 C20 1.449(2) . ?
C2 C6 1.437(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.346(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.317(3) . ?
C8 C9 1.401(3) . ?
C8 C13 1.402(3) . ?
C9 C10 1.397(3) . ?
C9 C14 1.515(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.381(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.394(3) . ?
C13 C17 1.519(3) . ?
C14 H14 1.0000 . ?
C14 C15 1.531(3) . ?
C14 C16 1.532(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 1.0000 . ?
C17 C18 1.532(3) . ?
C17 C19 1.534(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.398(3) . ?
C20 C25 1.402(3) . ?
C21 C22 1.394(3) . ?
C21 C26 1.523(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.380(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.380(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.398(3) . ?
C25 C29 1.512(3) . ?
C26 H26 1.0000 . ?
C26 C27 1.527(3) . ?
C26 C28 1.529(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 1.0000 . ?
C29 C30 1.515(3) . ?
C29 C31 1.523(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.404(4) . ?
C32 C34 1.398(4) 3_566 ?
C32 C35 1.689(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.383(5) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1A Ga1 Cl2A 109.78(10) . . ?
Cl1B Ga1 Cl2B 112.1(4) . . ?
Cl1B Ga1 Cl3B 106.7(4) . . ?
Cl2B Ga1 Cl3B 106.9(4) . . ?
Cl3A Ga1 Cl1A 107.30(11) . . ?
Cl3A Ga1 Cl2A 109.49(10) . . ?
C6 Ga1 Cl1A 116.72(12) . . ?
C6 Ga1 Cl1B 121.1(3) . . ?
C6 Ga1 Cl2A 106.65(11) . . ?
C6 Ga1 Cl2B 106.9(3) . . ?
C6 Ga1 Cl3A 106.73(12) . . ?
C6 Ga1 Cl3B 101.9(3) . . ?
C2 N1 C5 109.10(14) . . ?
C2 N1 C8 127.19(14) . . ?
C5 N1 C8 122.87(14) . . ?
C2 N2 C4 109.77(14) . . ?
C2 N2 C20 124.46(14) . . ?
C4 N2 C20 125.46(14) . . ?
N1 C2 N2 106.60(14) . . ?
N1 C2 C6 127.51(15) . . ?
N2 C2 C6 125.89(15) . . ?
N2 C4 H4 126.5 . . ?
C5 C4 N2 106.96(15) . . ?
C5 C4 H4 126.5 . . ?
N1 C5 H5 126.2 . . ?
C4 C5 N1 107.55(15) . . ?
C4 C5 H5 126.2 . . ?
C2 C6 Ga1 128.46(13) . . ?
C7 C6 Ga1 109.44(13) . . ?
C7 C6 C2 119.80(16) . . ?
O1 C7 C6 173.6(2) . . ?
C9 C8 N1 117.53(15) . . ?
C9 C8 C13 123.96(16) . . ?
C13 C8 N1 118.36(16) . . ?
C8 C9 C14 123.44(16) . . ?
C10 C9 C8 116.59(17) . . ?
C10 C9 C14 119.93(17) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 120.93(18) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.83(17) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.21(18) . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C17 123.29(16) . . ?
C12 C13 C8 116.45(17) . . ?
C12 C13 C17 120.19(17) . . ?
C9 C14 H14 107.9 . . ?
C9 C14 C15 111.37(16) . . ?
C9 C14 C16 110.68(16) . . ?
C15 C14 H14 107.9 . . ?
C15 C14 C16 110.88(17) . . ?
C16 C14 H14 107.9 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17 108.2 . . ?
C13 C17 C18 110.32(17) . . ?
C13 C17 C19 112.78(18) . . ?
C18 C17 H17 108.2 . . ?
C18 C17 C19 108.98(19) . . ?
C19 C17 H17 108.2 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N2 117.45(16) . . ?
C21 C20 C25 124.23(17) . . ?
C25 C20 N2 118.31(16) . . ?
C20 C21 C26 123.09(17) . . ?
C22 C21 C20 116.56(18) . . ?
C22 C21 C26 120.33(18) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 C21 121.1(2) . . ?
C23 C22 H22 119.5 . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.71(19) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 119.4 . . ?
C23 C24 C25 121.30(19) . . ?
C25 C24 H24 119.4 . . ?
C20 C25 C29 122.81(16) . . ?
C24 C25 C20 116.09(18) . . ?
C24 C25 C29 121.08(18) . . ?
C21 C26 H26 108.0 . . ?
C21 C26 C27 112.21(18) . . ?
C21 C26 C28 110.78(17) . . ?
C27 C26 H26 108.0 . . ?
C27 C26 C28 109.78(17) . . ?
C28 C26 H26 108.0 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29 107.8 . . ?
C25 C29 C30 110.01(18) . . ?
C25 C29 C31 111.8(2) . . ?
C30 C29 H29 107.8 . . ?
C30 C29 C31 111.4(3) . . ?
C31 C29 H29 107.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C35 119.9(3) . . ?
C34 C32 C33 116.5(3) 3_566 . ?
C34 C32 C35 123.6(3) 3_566 . ?
C32 C33 H33 119.2 . . ?
C34 C33 C32 121.7(3) . . ?
C34 C33 H33 119.2 . . ?
C32 C34 H34 119.1 3_566 . ?
C33 C34 C32 121.8(3) . 3_566 ?
C33 C34 H34 119.1 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 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 C2 C6 Ga1 -46.5(3) . . . . ?
N1 C2 C6 C7 152.70(18) . . . . ?
N1 C8 C9 C10 -177.74(15) . . . . ?
N1 C8 C9 C14 0.1(2) . . . . ?
N1 C8 C13 C12 177.59(15) . . . . ?
N1 C8 C13 C17 0.4(3) . . . . ?
N2 C2 C6 Ga1 133.90(16) . . . . ?
N2 C2 C6 C7 -26.9(3) . . . . ?
N2 C4 C5 N1 0.2(2) . . . . ?
N2 C20 C21 C22 -177.82(16) . . . . ?
N2 C20 C21 C26 0.4(3) . . . . ?
N2 C20 C25 C24 177.38(15) . . . . ?
N2 C20 C25 C29 -4.0(3) . . . . ?
C2 N1 C5 C4 -1.0(2) . . . . ?
C2 N1 C8 C9 -69.5(2) . . . . ?
C2 N1 C8 C13 114.73(19) . . . . ?
C2 N2 C4 C5 0.6(2) . . . . ?
C2 N2 C20 C21 98.1(2) . . . . ?
C2 N2 C20 C25 -80.8(2) . . . . ?
C4 N2 C2 N1 -1.20(19) . . . . ?
C4 N2 C2 C6 178.50(17) . . . . ?
C4 N2 C20 C21 -74.8(2) . . . . ?
C4 N2 C20 C25 106.2(2) . . . . ?
C5 N1 C2 N2 1.33(19) . . . . ?
C5 N1 C2 C6 -178.36(17) . . . . ?
C5 N1 C8 C9 98.9(2) . . . . ?
C5 N1 C8 C13 -76.9(2) . . . . ?
C8 N1 C2 N2 170.99(16) . . . . ?
C8 N1 C2 C6 -8.7(3) . . . . ?
C8 N1 C5 C4 -171.17(16) . . . . ?
C8 C9 C10 C11 1.0(3) . . . . ?
C8 C9 C14 C15 123.40(18) . . . . ?
C8 C9 C14 C16 -112.8(2) . . . . ?
C8 C13 C17 C18 97.1(2) . . . . ?
C8 C13 C17 C19 -140.8(2) . . . . ?
C9 C8 C13 C12 2.1(3) . . . . ?
C9 C8 C13 C17 -175.15(17) . . . . ?
C9 C10 C11 C12 0.2(3) . . . . ?
C10 C9 C14 C15 -58.8(2) . . . . ?
C10 C9 C14 C16 65.1(2) . . . . ?
C10 C11 C12 C13 -0.4(3) . . . . ?
C11 C12 C13 C8 -0.7(3) . . . . ?
C11 C12 C13 C17 176.58(18) . . . . ?
C12 C13 C17 C18 -80.0(2) . . . . ?
C12 C13 C17 C19 42.1(3) . . . . ?
C13 C8 C9 C10 -2.2(3) . . . . ?
C13 C8 C9 C14 175.70(16) . . . . ?
C14 C9 C10 C11 -176.99(17) . . . . ?
C20 N2 C2 N1 -175.12(15) . . . . ?
C20 N2 C2 C6 4.6(3) . . . . ?
C20 N2 C4 C5 174.46(16) . . . . ?
C20 C21 C22 C23 0.5(3) . . . . ?
C20 C21 C26 C27 137.92(19) . . . . ?
C20 C21 C26 C28 -99.0(2) . . . . ?
C20 C25 C29 C30 -102.3(3) . . . . ?
C20 C25 C29 C31 133.3(2) . . . . ?
C21 C20 C25 C24 -1.5(3) . . . . ?
C21 C20 C25 C29 177.08(17) . . . . ?
C21 C22 C23 C24 -1.5(3) . . . . ?
C22 C21 C26 C27 -43.9(3) . . . . ?
C22 C21 C26 C28 79.2(2) . . . . ?
C22 C23 C24 C25 1.0(3) . . . . ?
C23 C24 C25 C20 0.4(3) . . . . ?
C23 C24 C25 C29 -178.20(18) . . . . ?
C24 C25 C29 C30 76.3(3) . . . . ?
C24 C25 C29 C31 -48.1(3) . . . . ?
C25 C20 C21 C22 1.1(3) . . . . ?
C25 C20 C21 C26 179.32(17) . . . . ?
C26 C21 C22 C23 -177.82(19) . . . . ?
C32 C33 C34 C32 -0.7(4) . . . 3_566 ?
C34 C32 C33 C34 0.7(4) 3_566 . . . ?
C35 C32 C33 C34 -176.0(3) . . . . ?

_olex2_date_sample_data_collection 2021-05-10
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.834
####################################################################### 
# 
# 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_wf436_a
_database_code_depnum_ccdc_archive 'CCDC 2094751'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_audit_creation_date             2021-04-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H36 Au Cl N2 O'
_chemical_formula_sum            'C29 H36 Au Cl N2 O'
_chemical_formula_weight         661.01
_chemical_absolute_configuration rmad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C29 H36 Au Cl N2 O'
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'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
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'

_cell_length_a                   20.61099(13)
_cell_length_b                   12.54486(9)
_cell_length_c                   10.50093(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2715.14(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39680
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6140
_cell_measurement_theta_min      3.4990
_shelx_estimated_absorpt_T_max   0.322
_shelx_estimated_absorpt_T_min   0.043
_exptl_absorpt_coefficient_mu    11.258
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.004
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0650
1 0 0 0.0538
0 0 1 0.3386
0 0 -1 0.3464
0 -2 -1 0.2595
0 2 1 0.4490
1 -1 2 0.1902
-1 2 -2 0.2080
1 -2 2 0.2481
-1 6 -5 0.2198

_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.13
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
-1.0000 0.0000 -0.0000 -0.0723 0.0046 -0.0182
1.0000 -0.0000 0.0000 0.0723 -0.0046 0.0182
-0.0000 0.0000 1.0000 0.0034 0.1448 0.0232
0.0000 -0.0000 -1.0000 -0.0034 -0.1448 -0.0232
-0.0000 -2.0000 -1.0000 -0.0648 -0.1810 0.2119
0.0000 2.0000 1.0000 0.0648 0.1810 -0.2119
1.0000 -1.0000 2.0000 0.0484 0.2670 0.1821
-1.0000 2.0000 -2.0000 -0.0177 -0.2489 -0.2997
1.0000 -2.0000 2.0000 0.0177 0.2489 0.2997
-0.9999 6.0000 -5.0000 0.0950 -0.6111 -0.8395

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            47677
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.750
_diffrn_reflns_theta_min         4.125
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -81.00   9.00   1.00    1.00    --  -40.91 107.00-134.00   90
  2  ω     12.00  84.00   1.00    1.00    --   40.91-107.00 127.00   72
  3  ω    117.00 142.00   1.00    1.00    --  105.15 107.00-134.00   25
  4  ω     40.00 108.00   1.00    1.00    --  105.15-107.00 127.00   68
  5  ω     -4.00  21.00   1.00    1.00    --   34.00  93.00  28.54   25
  6  ω     -1.00  27.00   1.00    1.00    --   34.00  87.00  75.26   28
  7  ω   -114.00 -16.00   1.00    1.00    --  -40.91 -38.00 -60.00   98
  8  ω   -113.00 -16.00   1.00    1.00    --  -40.91 -38.00  90.00   97
  9  ω   -115.00 -16.00   1.00    1.00    --  -40.91 -38.00-150.00   99
 10  ω     28.00  92.00   1.00    1.00    --   40.91-125.00  90.00   64
 11  ω      5.00  30.00   1.00    1.00    --   40.91  87.00-164.71   25
 12  ω     14.00  40.00   1.00    1.00    --   46.00  79.00 -27.91   26
 13  ω     16.00  41.00   1.00    1.00    --   50.00  81.00  42.72   25
 14  ω     16.00  41.00   1.00    1.00    --   50.00  81.00  -5.51   25
 15  ω     16.00  41.00   1.00    1.00    --   50.00  82.00 -93.04   25
 16  ω     16.00  41.00   1.00    1.00    --   50.00  82.00-171.27   25
 17  ω     16.00  42.00   1.00    1.00    --   50.00  81.00  90.62   26
 18  ω     27.00  57.00   1.00    1.00    --   58.00  71.00 158.18   30
 19  ω     63.00 130.00   1.00    1.00    --   58.00  71.00 158.18   67
 20  ω     28.00  55.00   1.00    1.00    --   58.00  69.00-116.07   27
 21  ω     35.00  62.00   1.00    1.00    --   66.00  70.00 -90.31   27
 22  ω     92.00 119.00   1.00    1.00    --   66.00  70.00 -90.31   27
 23  ω     94.00 121.00   1.00    1.00    --   66.00  69.00  13.43   27
 24  ω     35.00  80.00   1.00    1.00    --   66.00  69.00  13.43   45
 25  ω     35.00  74.00   1.00    1.00    --   66.00  71.00  84.39   39
 26  ω     35.00  60.00   1.00    1.00    --   66.00  71.00 -48.89   25
 27  ω    112.00 140.00   1.00    1.00    --   66.00  71.00 -48.89   28
 28  ω     40.00  65.00   1.00    1.00    --   70.00  69.00-166.94   25
 29  ω     43.00  69.00   1.00    1.00    --   74.00  70.00 -24.26   26
 30  ω     43.00  74.00   1.00    1.00    --   74.00  69.00 146.01   31
 31  ω     47.00  73.00   1.00    1.00    --   78.00  69.00 101.84   26
 32  ω     52.00  80.00   1.00    1.00    --   82.00  67.00-137.29   28
 33  ω     51.00  80.00   1.00    1.00    --   82.00  70.00-162.33   29
 34  ω     54.00  81.00   1.00    1.00    --   82.00  63.00  -2.09   27
 35  ω     52.00  93.00   1.00    1.00    --   82.00  65.00  32.67   41
 36  ω     56.00  81.00   1.00    1.00    --   86.00  69.00 -68.40   25
 37  ω     55.00  84.00   1.00    1.00    --   86.00  69.00 175.98   29
 38  ω    114.00 158.00   1.00    1.00    --   86.00  66.00 107.72   44
 39  ω     57.00  83.00   1.00    1.00    --   86.00  66.00 107.72   26
 40  ω    124.00 152.00   1.00    1.00    --   86.00  69.00 175.98   28
 41  ω     63.00  90.00   1.00    1.00    --   90.00  55.00 -19.99   27
 42  ω     60.00  87.00   1.00    1.00    --   90.00  65.00-105.32   27
 43  ω    114.00 157.00   1.00    1.00    --  105.15  61.00 120.00   43
 44  ω     76.00 103.00   1.00    1.00    --  105.15  61.00 120.00   27
 45  ω     76.00 106.00   1.00    1.00    --  105.15  61.00  60.00   30
 46  ω    118.00 149.00   1.00    1.00    --  105.15  61.00  30.00   31
 47  ω     76.00 151.00   1.00    1.00    --  105.15  61.00-120.00   75
 48  ω     76.00 102.00   1.00    1.00    --  105.15  61.00  30.00   26
 49  ω    105.00 176.00   1.00    1.00    --  105.15 111.00-180.00   71
 50  ω     77.00 172.00   1.00    1.00    --  105.15  61.00-180.00   95
 51  ω     76.00 121.00   1.00    1.00    --  105.15  61.00 150.00   45
 52  ω    123.00 178.00   1.00    1.00    --  105.15 111.00 -60.00   55
 53  ω    117.00 169.00   1.00    1.00    --  105.15  61.00  90.00   52
 54  ω     80.00 106.00   1.00    1.00    --  105.15  61.00  90.00   26
 55  ω    105.00 158.00   1.00    1.00    --  105.15 111.00 120.00   53
 56  ω     34.00 105.00   1.00    1.00    --  105.15-111.00-120.00   71
 57  ω     79.00 149.00   1.00    1.00    --  105.15  61.00 -30.00   70
 58  ω     23.00 106.00   1.00    1.00    --  105.15 -94.00 -90.00   83
 59  ω    105.00 167.00   1.00    1.00    --  105.15 111.00 -90.00   62
 60  ω     76.00 127.00   1.00    1.00    --  105.15  61.00 -60.00   51
 61  ω     77.00 102.00   1.00    1.00    --  105.15  61.00   0.00   25
 62  ω    116.00 176.00   1.00    1.00    --  105.15  61.00   0.00   60
 63  ω     76.00 161.00   1.00    1.00    --  105.15  61.00 -90.00   85
 64  ω     34.00  96.00   1.00    1.00    --  105.15 -94.00 -30.00   62
 65  ω     78.00 137.00   1.00    1.00    --  105.15  61.00-150.00   59
 66  ω     30.00 103.00   1.00    1.00    --  105.15-111.00  60.00   73
 67  ω    119.00 177.00   1.00    1.00    --  105.15  61.00  60.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0723330000
_diffrn_orient_matrix_UB_12      0.0306997000
_diffrn_orient_matrix_UB_13      0.0033782000
_diffrn_orient_matrix_UB_21      -0.0046224000
_diffrn_orient_matrix_UB_22      0.0180686000
_diffrn_orient_matrix_UB_23      0.1448361000
_diffrn_orient_matrix_UB_31      0.0181737000
_diffrn_orient_matrix_UB_32      -0.1175451000
_diffrn_orient_matrix_UB_33      0.0232132000
_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         0.882
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                5353
_reflns_number_total             5359
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         1.960
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 
;
 Flack x determined using 2450 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(10)
_refine_ls_extinction_coef       0.00087(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5359
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0599P)²+0.9067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0827
_refine_special_details          ?
_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:
 C14(H14), C17(H17), C26(H26), C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C22(H22), C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.48492(2) 0.74051(2) 0.38696(8) 0.02445(12) Uani 1 1 d . . . . .
Cl1 Cl 0.40401(6) 0.86380(13) 0.40768(15) 0.0368(3) Uani 1 1 d . . . . .
O1 O 0.5057(2) 0.4642(4) 0.2909(5) 0.0390(11) Uani 1 1 d . . . . .
N1 N 0.67201(17) 0.5730(3) 0.3691(4) 0.0213(8) Uani 1 1 d . . . . .
N2 N 0.6529(3) 0.7361(4) 0.4268(5) 0.0210(10) Uani 1 1 d . . . . .
C2 C 0.6245(2) 0.6467(4) 0.3843(6) 0.0217(8) Uani 1 1 d . . . . .
C4 C 0.73164(19) 0.6190(4) 0.3994(6) 0.0251(10) Uani 1 1 d . . . . .
H4 H 0.772865 0.585302 0.394976 0.030 Uiso 1 1 calc R U . . .
C5 C 0.7200(3) 0.7190(5) 0.4359(6) 0.0257(11) Uani 1 1 d . . . . .
H5 H 0.751458 0.769534 0.462984 0.031 Uiso 1 1 calc R U . . .
C6 C 0.5572(2) 0.6316(5) 0.3624(5) 0.0240(11) Uani 1 1 d . . . . .
C7 C 0.5323(2) 0.5405(5) 0.3237(5) 0.0298(12) Uani 1 1 d . . . . .
C8 C 0.6628(2) 0.4688(4) 0.3151(5) 0.0235(11) Uani 1 1 d . . . . .
C9 C 0.65401(19) 0.3811(4) 0.3961(6) 0.0251(9) Uani 1 1 d . . . . .
C10 C 0.6421(3) 0.2829(5) 0.3383(6) 0.0340(12) Uani 1 1 d . . . . .
H10 H 0.636917 0.221457 0.390217 0.041 Uiso 1 1 calc R U . . .
C11 C 0.6377(3) 0.2724(5) 0.2075(7) 0.0351(14) Uani 1 1 d . . . . .
H11 H 0.627976 0.205143 0.170716 0.042 Uiso 1 1 calc R U . . .
C12 C 0.6475(2) 0.3610(5) 0.1301(5) 0.0292(11) Uani 1 1 d . . . . .
H12 H 0.645182 0.353196 0.040229 0.035 Uiso 1 1 calc R U . . .
C13 C 0.6607(2) 0.4608(5) 0.1819(5) 0.0253(11) Uani 1 1 d . . . . .
C14 C 0.6544(3) 0.3907(5) 0.5404(5) 0.0288(12) Uani 1 1 d . . . . .
H14 H 0.680543 0.455031 0.563530 0.035 Uiso 1 1 calc R U . . .
C15 C 0.5857(3) 0.4066(7) 0.5920(7) 0.0522(19) Uani 1 1 d . . . . .
H15A H 0.567448 0.472576 0.557244 0.078 Uiso 1 1 calc R U . . .
H15B H 0.587121 0.411174 0.685126 0.078 Uiso 1 1 calc R U . . .
H15C H 0.558489 0.346107 0.566699 0.078 Uiso 1 1 calc R U . . .
C16 C 0.6857(3) 0.2932(6) 0.6049(7) 0.0411(14) Uani 1 1 d . . . . .
H16A H 0.658654 0.230168 0.589991 0.062 Uiso 1 1 calc R U . . .
H16B H 0.689252 0.306112 0.696703 0.062 Uiso 1 1 calc R U . . .
H16C H 0.728969 0.281376 0.569129 0.062 Uiso 1 1 calc R U . . .
C17 C 0.6728(3) 0.5551(5) 0.0928(5) 0.0290(12) Uani 1 1 d . . . . .
H17 H 0.681153 0.619678 0.146203 0.035 Uiso 1 1 calc R U . . .
C18 C 0.6127(3) 0.5759(8) 0.0122(8) 0.056(2) Uani 1 1 d . . . . .
H18A H 0.601185 0.511038 -0.034666 0.083 Uiso 1 1 calc R U . . .
H18B H 0.621613 0.633586 -0.048242 0.083 Uiso 1 1 calc R U . . .
H18C H 0.576535 0.596469 0.067650 0.083 Uiso 1 1 calc R U . . .
C19 C 0.7325(3) 0.5361(6) 0.0085(7) 0.0456(17) Uani 1 1 d . . . . .
H19A H 0.769599 0.516788 0.062057 0.068 Uiso 1 1 calc R U . . .
H19B H 0.742487 0.601222 -0.039033 0.068 Uiso 1 1 calc R U . . .
H19C H 0.723402 0.477996 -0.051328 0.068 Uiso 1 1 calc R U . . .
C20 C 0.6229(2) 0.8385(5) 0.4465(5) 0.0212(10) Uani 1 1 d . . . . .
C21 C 0.6049(2) 0.8686(5) 0.5692(5) 0.0257(11) Uani 1 1 d . . . . .
C22 C 0.5790(2) 0.9703(5) 0.5851(5) 0.0279(11) Uani 1 1 d . . . . .
H22 H 0.567602 0.993849 0.668173 0.033 Uiso 1 1 calc R U . . .
C23 C 0.5696(2) 1.0373(5) 0.4832(6) 0.0295(11) Uani 1 1 d . . . . .
H23 H 0.550786 1.105618 0.496152 0.035 Uiso 1 1 calc R U . . .
C24 C 0.5874(2) 1.0055(4) 0.3611(5) 0.0260(11) Uani 1 1 d . . . . .
H24 H 0.580449 1.052381 0.291378 0.031 Uiso 1 1 calc R U . . .
C25 C 0.6155(2) 0.9056(5) 0.3397(5) 0.0234(10) Uani 1 1 d . . . . .
C26 C 0.6127(2) 0.7946(5) 0.6825(5) 0.0280(11) Uani 1 1 d . . . . .
H26 H 0.625352 0.722362 0.650781 0.034 Uiso 1 1 calc R U . . .
C27 C 0.6661(3) 0.8357(6) 0.7716(6) 0.0401(15) Uani 1 1 d . . . . .
H27A H 0.707115 0.840512 0.724793 0.060 Uiso 1 1 calc R U . . .
H27B H 0.671130 0.786447 0.843390 0.060 Uiso 1 1 calc R U . . .
H27C H 0.654141 0.906398 0.803653 0.060 Uiso 1 1 calc R U . . .
C28 C 0.5483(3) 0.7854(6) 0.7538(6) 0.0350(13) Uani 1 1 d . . . . .
H28A H 0.537391 0.854435 0.791868 0.052 Uiso 1 1 calc R U . . .
H28B H 0.552272 0.731636 0.821048 0.052 Uiso 1 1 calc R U . . .
H28C H 0.514079 0.764289 0.694223 0.052 Uiso 1 1 calc R U . . .
C29 C 0.6353(3) 0.8750(5) 0.2064(5) 0.0267(11) Uani 1 1 d . . . . .
H29 H 0.656979 0.803746 0.210223 0.032 Uiso 1 1 calc R U . . .
C30 C 0.6836(3) 0.9550(5) 0.1526(6) 0.0348(13) Uani 1 1 d . . . . .
H30A H 0.662154 1.023976 0.140681 0.052 Uiso 1 1 calc R U . . .
H30B H 0.699947 0.929282 0.070497 0.052 Uiso 1 1 calc R U . . .
H30C H 0.719960 0.963264 0.212040 0.052 Uiso 1 1 calc R U . . .
C31 C 0.5766(3) 0.8657(7) 0.1182(6) 0.0428(16) Uani 1 1 d . . . . .
H31A H 0.557148 0.936293 0.106222 0.064 Uiso 1 1 calc R U . . .
H31B H 0.544565 0.817571 0.156219 0.064 Uiso 1 1 calc R U . . .
H31C H 0.590469 0.837385 0.035606 0.064 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
Au1 Cl1 2.2849(13) . ?
Au1 C6 2.038(5) . ?
O1 C7 1.156(8) . ?
N1 C2 1.356(6) . ?
N1 C4 1.395(6) . ?
N1 C8 1.437(7) . ?
N2 C2 1.343(7) . ?
N2 C5 1.402(8) . ?
N2 C20 1.441(7) . ?
C2 C6 1.418(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.334(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.317(8) . ?
C8 C9 1.403(8) . ?
C8 C13 1.403(7) . ?
C9 C10 1.395(9) . ?
C9 C14 1.520(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(10) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.391(8) . ?
C13 C17 1.529(8) . ?
C14 H14 1.0000 . ?
C14 C15 1.529(8) . ?
C14 C16 1.539(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 1.0000 . ?
C17 C18 1.524(8) . ?
C17 C19 1.533(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.393(8) . ?
C20 C25 1.411(8) . ?
C21 C22 1.393(8) . ?
C21 C26 1.517(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.375(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.392(8) . ?
C24 H24 0.9500 . ?
C24 C25 1.400(8) . ?
C25 C29 1.508(7) . ?
C26 H26 1.0000 . ?
C26 C27 1.534(8) . ?
C26 C28 1.528(8) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 1.0000 . ?
C29 C30 1.524(8) . ?
C29 C31 1.527(8) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Au1 Cl1 178.17(16) . . ?
C2 N1 C4 109.1(4) . . ?
C2 N1 C8 124.8(4) . . ?
C4 N1 C8 125.7(4) . . ?
C2 N2 C5 109.0(5) . . ?
C2 N2 C20 127.2(5) . . ?
C5 N2 C20 123.4(5) . . ?
N1 C2 C6 126.6(5) . . ?
N2 C2 N1 107.1(4) . . ?
N2 C2 C6 126.3(5) . . ?
N1 C4 H4 126.4 . . ?
C5 C4 N1 107.3(4) . . ?
C5 C4 H4 126.4 . . ?
N2 C5 H5 126.2 . . ?
C4 C5 N2 107.6(5) . . ?
C4 C5 H5 126.2 . . ?
C2 C6 Au1 127.2(4) . . ?
C7 C6 Au1 109.6(3) . . ?
C7 C6 C2 123.1(5) . . ?
O1 C7 C6 174.6(6) . . ?
C9 C8 N1 119.4(4) . . ?
C13 C8 N1 117.6(5) . . ?
C13 C8 C9 123.0(5) . . ?
C8 C9 C14 122.8(5) . . ?
C10 C9 C8 116.8(6) . . ?
C10 C9 C14 120.3(5) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 C9 121.8(6) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.7(6) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.2(5) . . ?
C13 C12 H12 119.4 . . ?
C8 C13 C17 123.3(5) . . ?
C12 C13 C8 117.4(5) . . ?
C12 C13 C17 119.3(5) . . ?
C9 C14 H14 108.0 . . ?
C9 C14 C15 111.0(5) . . ?
C9 C14 C16 112.2(5) . . ?
C15 C14 H14 108.0 . . ?
C15 C14 C16 109.6(5) . . ?
C16 C14 H14 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17 108.2 . . ?
C13 C17 C19 111.3(5) . . ?
C18 C17 C13 109.8(5) . . ?
C18 C17 H17 108.2 . . ?
C18 C17 C19 111.0(5) . . ?
C19 C17 H17 108.2 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N2 119.3(5) . . ?
C21 C20 C25 123.0(5) . . ?
C25 C20 N2 117.6(5) . . ?
C20 C21 C22 117.5(5) . . ?
C20 C21 C26 122.1(5) . . ?
C22 C21 C26 120.5(5) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 C21 121.4(5) . . ?
C23 C22 H22 119.3 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.3(5) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.5 . . ?
C23 C24 C25 120.9(5) . . ?
C25 C24 H24 119.5 . . ?
C20 C25 C29 123.9(5) . . ?
C24 C25 C20 116.8(5) . . ?
C24 C25 C29 119.3(5) . . ?
C21 C26 H26 108.7 . . ?
C21 C26 C27 110.4(5) . . ?
C21 C26 C28 109.8(5) . . ?
C27 C26 H26 108.7 . . ?
C28 C26 H26 108.7 . . ?
C28 C26 C27 110.4(5) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29 108.1 . . ?
C25 C29 C30 110.7(5) . . ?
C25 C29 C31 111.6(5) . . ?
C30 C29 H29 108.1 . . ?
C30 C29 C31 110.1(5) . . ?
C31 C29 H29 108.1 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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 C2 C6 Au1 179.1(4) . . . . ?
N1 C2 C6 C7 0.3(10) . . . . ?
N1 C4 C5 N2 -0.7(7) . . . . ?
N1 C8 C9 C10 177.0(4) . . . . ?
N1 C8 C9 C14 -0.5(6) . . . . ?
N1 C8 C13 C12 -175.9(4) . . . . ?
N1 C8 C13 C17 4.8(7) . . . . ?
N2 C2 C6 Au1 0.7(9) . . . . ?
N2 C2 C6 C7 -178.1(6) . . . . ?
N2 C20 C21 C22 176.8(5) . . . . ?
N2 C20 C21 C26 -3.3(8) . . . . ?
N2 C20 C25 C24 -178.7(4) . . . . ?
N2 C20 C25 C29 2.0(7) . . . . ?
C2 N1 C4 C5 1.5(7) . . . . ?
C2 N1 C8 C9 -97.2(6) . . . . ?
C2 N1 C8 C13 80.6(6) . . . . ?
C2 N2 C5 C4 -0.4(7) . . . . ?
C2 N2 C20 C21 100.1(7) . . . . ?
C2 N2 C20 C25 -82.4(7) . . . . ?
C4 N1 C2 N2 -1.8(7) . . . . ?
C4 N1 C2 C6 179.6(6) . . . . ?
C4 N1 C8 C9 91.0(6) . . . . ?
C4 N1 C8 C13 -91.2(6) . . . . ?
C5 N2 C2 N1 1.3(7) . . . . ?
C5 N2 C2 C6 180.0(6) . . . . ?
C5 N2 C20 C21 -87.8(7) . . . . ?
C5 N2 C20 C25 89.7(7) . . . . ?
C8 N1 C2 N2 -174.6(5) . . . . ?
C8 N1 C2 C6 6.7(9) . . . . ?
C8 N1 C4 C5 174.3(5) . . . . ?
C8 C9 C10 C11 -1.4(8) . . . . ?
C8 C9 C14 C15 92.8(6) . . . . ?
C8 C9 C14 C16 -144.3(5) . . . . ?
C8 C13 C17 C18 -118.9(6) . . . . ?
C8 C13 C17 C19 117.8(6) . . . . ?
C9 C8 C13 C12 1.8(7) . . . . ?
C9 C8 C13 C17 -177.5(4) . . . . ?
C9 C10 C11 C12 2.3(10) . . . . ?
C10 C9 C14 C15 -84.7(7) . . . . ?
C10 C9 C14 C16 38.3(7) . . . . ?
C10 C11 C12 C13 -1.1(9) . . . . ?
C11 C12 C13 C8 -0.9(8) . . . . ?
C11 C12 C13 C17 178.5(5) . . . . ?
C12 C13 C17 C18 61.8(7) . . . . ?
C12 C13 C17 C19 -61.6(7) . . . . ?
C13 C8 C9 C10 -0.7(7) . . . . ?
C13 C8 C9 C14 -178.2(4) . . . . ?
C14 C9 C10 C11 176.2(6) . . . . ?
C20 N2 C2 N1 174.3(5) . . . . ?
C20 N2 C2 C6 -7.0(10) . . . . ?
C20 N2 C5 C4 -173.7(5) . . . . ?
C20 C21 C22 C23 2.0(8) . . . . ?
C20 C21 C26 C27 110.6(6) . . . . ?
C20 C21 C26 C28 -127.4(6) . . . . ?
C20 C25 C29 C30 -122.8(6) . . . . ?
C20 C25 C29 C31 114.2(6) . . . . ?
C21 C20 C25 C24 -1.3(7) . . . . ?
C21 C20 C25 C29 179.4(5) . . . . ?
C21 C22 C23 C24 -1.6(8) . . . . ?
C22 C21 C26 C27 -69.5(6) . . . . ?
C22 C21 C26 C28 52.5(7) . . . . ?
C22 C23 C24 C25 -0.4(8) . . . . ?
C23 C24 C25 C20 1.8(7) . . . . ?
C23 C24 C25 C29 -178.9(5) . . . . ?
C24 C25 C29 C30 57.9(6) . . . . ?
C24 C25 C29 C31 -65.0(7) . . . . ?
C25 C20 C21 C22 -0.5(8) . . . . ?
C25 C20 C21 C26 179.4(5) . . . . ?
C26 C21 C22 C23 -177.9(5) . . . . ?

_olex2_date_sample_data_collection 2021-04-16
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.531
_oxdiff_exptl_absorpt_empirical_full_min 0.523
