# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_exp_1049
_database_code_depnum_ccdc_archive 'CCDC 2180629'
loop_
_audit_author_name
_audit_author_address
'Sunewang Rixin Wang'
;East China Normal University
China
;
_audit_update_record             
;
2022-06-21 deposited with the CCDC.	2022-10-02 downloaded from the CCDC.
;
_audit_creation_date             2019-11-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         '2(C26 H19 Br O3)'
_chemical_formula_sum            'C52 H38 Br2 O6'
_chemical_formula_weight         918.68
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Br -0.67402 1.33011 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090
41.43280 2.95569992065
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_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_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   11.52440(10)
_cell_length_b                   14.4273(2)
_cell_length_c                   25.8302(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.8350(10)
_cell_angle_gamma                90
_cell_volume                     4231.57(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    48309
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.0940
_cell_measurement_theta_min      4.6180
_exptl_absorpt_coefficient_mu    2.847
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4419
_exptl_crystal_description       block
_exptl_crystal_F_000             1871.6656
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            121216
_diffrn_reflns_theta_full        67.0738
_diffrn_reflns_theta_max         67.07
_diffrn_reflns_theta_min         3.89
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9914
_diffrn_measured_fraction_theta_max 0.9914
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00   7.00   1.00    1.00    --    0.00 -12.00  27.00   26
  2  ω    -28.00  -2.00   1.00    1.00    --    0.00  12.00-160.00   26
  3  ω    100.00 126.00   1.00    1.00    --   95.80  12.00-160.00   26
  4  ω     47.00  81.00   1.00    1.00    --   95.80 -12.00  27.00   34
  5  ω    -21.00  27.00   1.00    1.00    --    0.00  57.00 -60.00   48
  6  ω     36.00  62.00   1.00    1.00    --    0.00  57.00-150.00   26
  7  ω    -23.00  30.00   1.00    1.00    --    0.00 -77.00  30.00   53
  8  ω     50.00  75.00   1.00    1.00    --    0.00  38.00-180.00   25
  9  ω     33.00  88.00   1.00    1.00    --    0.00  38.00 -30.00   55
 10  ω    -89.00 -34.00   1.00    1.00    --    0.00 -77.00  30.00   55
 11  ω    -19.00  87.00   1.00    1.00    --    0.00  38.00-120.00  106
 12  ω    -16.00  13.00   1.00    1.00    --    0.00  57.00-150.00   29
 13  ω    -23.00  53.00   1.00    1.00    --    0.00  57.00 120.00   76
 14  ω    -19.00   8.00   1.00    1.00    --    0.00  38.00 -60.00   27
 15  ω     19.00  84.00   1.00    1.00    --    0.00  38.00 -60.00   65
 16  ω    -15.00  12.00   1.00    1.00    --    0.00  38.00 -30.00   27
 17  ω     57.00  87.00   1.00    1.00    --    0.00  57.00 120.00   30
 18  ω    -23.00  79.00   1.00    1.00    --    0.00  57.00  30.00  102
 19  ω     32.00  59.00   1.00    1.00    --    0.00  57.00 -60.00   27
 20  ω    -18.00  22.00   1.00    1.00    --    0.00  38.00-180.00   40
 21  ω     35.00  61.00   1.00    1.00    --    0.00  12.00-160.00   26
 22  ω    113.00 184.00   1.00    1.00    --   95.80  82.00-150.00   71
 23  ω     63.00  90.00   1.00    1.00    --   95.80  82.00-150.00   27
 24  ω     63.00  89.00   1.00    1.00    --   95.80  82.00  60.00   26
 25  ω    152.00 177.00   1.00    1.00    --   95.80  82.00 150.00   25
 26  ω    125.00 165.00   1.00    1.00    --   95.80  76.00  52.67   40
 27  ω     65.00  90.00   1.00    1.00    --   95.80  76.00  52.67   25
 28  ω     95.00 121.00   1.00    1.00    --   95.80  82.00 150.00   26
 29  ω     63.00  89.00   1.00    1.00    --   95.80  82.00 -30.00   26
 30  ω     12.00  38.00   1.00    1.00    --   95.80 -82.00  30.00   26
 31  ω     65.00  90.00   1.00    1.00    --   95.80  77.00-150.00   25
 32  ω     75.00 105.00   1.00    1.00    --   95.80  45.00 -90.00   30
 33  ω    139.00 171.00   1.00    1.00    --   95.80  61.00-180.00   32
 34  ω     68.00  94.00   1.00    1.00    --   95.80  69.00-113.06   26
 35  ω      6.00 128.00   1.00    1.00    --   95.80 -82.00-180.00  122
 36  ω    157.00 185.00   1.00    1.00    --   95.80  82.00  30.00   28
 37  ω     69.00  95.00   1.00    1.00    --   95.80  65.00 -27.01   26
 38  ω    145.00 171.00   1.00    1.00    --   95.80  77.00-101.32   26
 39  ω     63.00  89.00   1.00    1.00    --   95.80  82.00 150.00   26
 40  ω     65.00  91.00   1.00    1.00    --   95.80  77.00-101.32   26
 41  ω     63.00  90.00   1.00    1.00    --   95.80  81.00  98.23   27
 42  ω     65.00  91.00   1.00    1.00    --   95.80  77.00  85.75   26
 43  ω     69.00 180.00   1.00    1.00    --   95.80  66.00 148.69  111
 44  ω     63.00  88.00   1.00    1.00    --   95.80  82.00-120.00   25
 45  ω    102.00 146.00   1.00    1.00    --   95.80  81.00  98.23   44
 46  ω    152.00 185.00   1.00    1.00    --   95.80  81.00  98.23   33
 47  ω     65.00  91.00   1.00    1.00    --   95.80  77.00 -90.00   26
 48  ω     65.00 160.00   1.00    1.00    --   95.80  77.00  30.00   95
 49  ω     72.00  98.00   1.00    1.00    --   95.80  57.00-114.45   26
 50  ω     72.00 184.00   1.00    1.00    --   95.80  61.00 -30.00  112
 51  ω     69.00  95.00   1.00    1.00    --   95.80  66.00  92.75   26
 52  ω     52.00 125.00   1.00    1.00    --   95.80 -82.00 150.00   73
 53  ω     64.00 184.00   1.00    1.00    --   95.80  79.00-171.33  120
 54  ω     65.00  91.00   1.00    1.00    --   95.80  77.00  90.00   26
 55  ω     65.00 175.00   1.00    1.00    --   95.80  77.00  19.08  110
 56  ω    158.00 183.00   1.00    1.00    --   95.80  82.00 -30.00   25
 57  ω     65.00  91.00   1.00    1.00    --   95.80  76.00  -4.02   26
 58  ω     52.00  78.00   1.00    1.00    --   95.80 -82.00  30.00   26
 59  ω     97.00 127.00   1.00    1.00    --   95.80 -82.00  30.00   30
 60  ω     65.00  90.00   1.00    1.00    --   95.80  77.00-180.00   25
 61  ω     65.00  91.00   1.00    1.00    --   95.80  77.00 150.00   26
 62  ω     71.00  97.00   1.00    1.00    --   95.80  61.00-180.00   26
 63  ω     82.00 128.00   1.00    1.00    --   95.80 -82.00-120.00   46
 64  ω     74.00 184.00   1.00    1.00    --   95.80  50.00 -73.29  110
 65  ω     74.00 108.00   1.00    1.00    --   95.80  51.00-124.42   34
 66  ω    122.00 184.00   1.00    1.00    --   95.80  51.00-124.42   62
 67  ω     63.00 108.00   1.00    1.00    --   95.80  82.00 -90.00   45
 68  ω     68.00  93.00   1.00    1.00    --   95.80  70.00-178.01   25
 69  ω    146.00 171.00   1.00    1.00    --   95.80  76.00 -69.81   25
 70  ω     49.00  76.00   1.00    1.00    --   95.80 -82.00-120.00   27
 71  ω     65.00  91.00   1.00    1.00    --   95.80  77.00-120.00   26
 72  ω     66.00  92.00   1.00    1.00    --   95.80  76.00 -69.81   26
 73  ω     70.00 109.00   1.00    1.00    --   95.80  63.00   7.07   39
 74  ω     72.00  98.00   1.00    1.00    --   95.80  55.00  84.28   26
 75  ω     69.00  95.00   1.00    1.00    --   95.80  68.00 -11.90   26
 76  ω    124.00 182.00   1.00    1.00    --   95.80  68.00 -11.90   58
 77  ω     67.00 102.00   1.00    1.00    --   95.80  72.00 118.30   35
 78  ω     68.00 124.00   1.00    1.00    --   95.80  68.00  94.46   56
 79  ω     66.00 117.00   1.00    1.00    --   95.80  77.00 -66.11   51
 80  ω     21.00  46.00   1.00    1.00    --   95.80 -82.00 150.00   25
 81  ω     63.00  88.00   1.00    1.00    --   95.80  82.00   0.00   25
 82  ω     65.00 185.00   1.00    1.00    --   95.80  77.00 120.00  120
 83  ω    107.00 183.00   1.00    1.00    --   95.80  82.00  60.00   76
 84  ω     65.00  91.00   1.00    1.00    --   95.80  77.00 -30.00   26
 85  ω    110.00 173.00   1.00    1.00    --   95.80  77.00  85.75   63
 86  ω     65.00 132.00   1.00    1.00    --   95.80  77.00 -60.00   67
 87  ω     64.00 128.00   1.00    1.00    --   95.80 -82.00 -30.00   64
 88  ω     49.00 124.00   1.00    1.00    --   95.80 -82.00  60.00   75
 89  ω     63.00  88.00   1.00    1.00    --   95.80  82.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0671616000
_diffrn_orient_matrix_UB_12      0.0927461000
_diffrn_orient_matrix_UB_13      0.0035534000
_diffrn_orient_matrix_UB_21      -0.1178624000
_diffrn_orient_matrix_UB_22      0.0529417000
_diffrn_orient_matrix_UB_23      -0.0081825000
_diffrn_orient_matrix_UB_31      0.0033009000
_diffrn_orient_matrix_UB_32      0.0017538000
_diffrn_orient_matrix_UB_33      0.0598429000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                7120
_reflns_number_total             7490
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.8815
_refine_diff_density_min         -0.9224
_refine_diff_density_rms         0.0925
_refine_ls_d_res_high            0.8370
_refine_ls_d_res_low             11.3550
_refine_ls_goodness_of_fit_ref   1.0446
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.0446
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0177P)²+15.9559P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1109
_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:
 C9(H9), C10(H10), C35(H35), C36(H36)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C39(H39), C40(H40), C41(H41), C42(H42),
 C43(H43), C48(H48), C50(H50), C51(H51), C52(H52)
2.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C45(H45a,H45b,H45c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
Br1 Br 0.72668(4) 0.96311(3) 0.989596(16) 0.04267(14) Uani 1.000000 .
O1 O 0.3409(2) 0.71614(17) 0.70438(11) 0.0337(6) Uani 1.000000 .
O2 O 0.3550(2) 0.56252(16) 0.71368(9) 0.0262(5) Uani 1.000000 .
O3 O 0.7437(2) 0.73851(18) 0.82413(9) 0.0287(5) Uani 1.000000 .
C1 C 0.4193(3) 0.6880(3) 0.53890(14) 0.0272(7) Uani 1.000000 .
C2 C 0.3856(3) 0.7013(3) 0.48559(14) 0.0302(8) Uani 1.000000 .
C3 C 0.4482(3) 0.7614(3) 0.45866(14) 0.0305(8) Uani 1.000000 .
C4 C 0.5431(3) 0.8094(3) 0.48582(14) 0.0304(8) Uani 1.000000 .
C5 C 0.5777(3) 0.7966(3) 0.53906(14) 0.0283(8) Uani 1.000000 .
C6 C 0.5178(3) 0.7342(2) 0.56650(13) 0.0235(7) Uani 1.000000 .
C7 C 0.5553(3) 0.7164(2) 0.62145(13) 0.0232(7) Uani 1.000000 .
C8 C 0.5844(3) 0.7008(2) 0.66720(13) 0.0226(7) Uani 1.000000 .
C9 C 0.6135(3) 0.6832(2) 0.72293(12) 0.0211(7) Uani 1.000000 .
C10 C 0.5687(3) 0.7488(2) 0.76066(13) 0.0209(7) Uani 1.000000 .
C11 C 0.5182(3) 0.6503(2) 0.75315(12) 0.0186(6) Uani 1.000000 .
C12 C 0.5458(3) 0.5791(2) 0.79546(12) 0.0193(6) Uani 1.000000 .
C13 C 0.6189(3) 0.5041(2) 0.79003(13) 0.0229(7) Uani 1.000000 .
C14 C 0.6394(3) 0.4361(2) 0.82885(14) 0.0280(8) Uani 1.000000 .
C15 C 0.5869(3) 0.4431(2) 0.87308(14) 0.0291(8) Uani 1.000000 .
C16 C 0.5146(3) 0.5174(2) 0.87881(13) 0.0269(7) Uani 1.000000 .
C17 C 0.4943(3) 0.5857(2) 0.84028(13) 0.0230(7) Uani 1.000000 .
C18 C 0.3951(3) 0.6491(2) 0.72152(12) 0.0194(7) Uani 1.000000 .
C19 C 0.2386(3) 0.5548(3) 0.68182(14) 0.0295(8) Uani 1.000000 .
C20 C 0.6455(3) 0.7723(2) 0.81158(13) 0.0214(7) Uani 1.000000 .
C21 C 0.5963(3) 0.8378(2) 0.84717(12) 0.0208(7) Uani 1.000000 .
C22 C 0.6702(3) 0.8669(2) 0.89277(13) 0.0241(7) Uani 1.000000 .
C23 C 0.6266(3) 0.9268(2) 0.92642(14) 0.0279(8) Uani 1.000000 .
C24 C 0.5119(3) 0.9598(3) 0.91598(14) 0.0290(8) Uani 1.000000 .
C25 C 0.4396(3) 0.9305(3) 0.87101(14) 0.0294(8) Uani 1.000000 .
C26 C 0.4800(3) 0.8699(2) 0.83657(13) 0.0243(7) Uani 1.000000 .
Br2 Br 1.24366(4) 0.51045(3) 0.996066(15) 0.03622(12) Uani 1.000000 .
O4 O 0.8555(2) 0.91942(16) 0.72731(9) 0.0268(5) Uani 1.000000 .
O5 O 0.8469(2) 0.76719(16) 0.70853(9) 0.0262(5) Uani 1.000000 .
O6 O 1.2447(2) 0.73918(19) 0.83300(10) 0.0321(6) Uani 1.000000 .
C27 C 0.9056(3) 0.7713(2) 0.55550(14) 0.0278(8) Uani 1.000000 .
C28 C 0.8686(3) 0.7666(3) 0.50176(14) 0.0302(8) Uani 1.000000 .
C29 C 0.9508(4) 0.7583(3) 0.46872(14) 0.0332(9) Uani 1.000000 .
C30 C 1.0695(4) 0.7533(3) 0.48939(15) 0.0352(9) Uani 1.000000 .
C31 C 1.1073(3) 0.7588(3) 0.54281(15) 0.0303(8) Uani 1.000000 .
C32 C 1.0255(3) 0.7697(2) 0.57667(13) 0.0228(7) Uani 1.000000 .
C33 C 1.0625(3) 0.7790(2) 0.63214(13) 0.0234(7) Uani 1.000000 .
C34 C 1.0890(3) 0.7883(2) 0.67870(14) 0.0238(7) Uani 1.000000 .
C35 C 1.1150(3) 0.7998(2) 0.73464(13) 0.0233(7) Uani 1.000000 .
C36 C 1.0690(3) 0.7317(2) 0.77039(13) 0.0225(7) Uani 1.000000 .
C37 C 1.0180(3) 0.8289(2) 0.76472(12) 0.0200(7) Uani 1.000000 .
C38 C 1.0430(3) 0.8992(2) 0.80795(13) 0.0216(7) Uani 1.000000 .
C39 C 1.0993(3) 0.9822(2) 0.80073(14) 0.0271(7) Uani 1.000000 .
C40 C 1.1156(3) 1.0487(3) 0.84000(15) 0.0335(8) Uani 1.000000 .
C41 C 1.0762(3) 1.0331(3) 0.88691(15) 0.0329(8) Uani 1.000000 .
C42 C 1.0208(3) 0.9501(3) 0.89462(14) 0.0336(8) Uani 1.000000 .
C43 C 1.0038(3) 0.8839(2) 0.85514(13) 0.0271(7) Uani 1.000000 .
C44 C 0.8971(3) 0.8326(2) 0.73101(12) 0.0198(7) Uani 1.000000 .
C45 C 0.7435(3) 0.9314(3) 0.69282(14) 0.0311(8) Uani 1.000000 .
C46 C 1.1471(3) 0.7046(2) 0.82041(13) 0.0241(7) Uani 1.000000 .
C47 C 1.1013(3) 0.6358(2) 0.85520(13) 0.0226(7) Uani 1.000000 .
C48 C 1.1788(3) 0.6054(2) 0.89962(13) 0.0249(7) Uani 1.000000 .
C49 C 1.1389(3) 0.5442(2) 0.93377(14) 0.0270(7) Uani 1.000000 .
C50 C 1.0251(3) 0.5111(3) 0.92506(14) 0.0304(8) Uani 1.000000 .
C51 C 0.9485(3) 0.5420(3) 0.88101(14) 0.0296(8) Uani 1.000000 .
C52 C 0.9857(3) 0.6041(2) 0.84615(13) 0.0258(7) Uani 1.000000 .
H24 H 0.4844(3) 1.0009(3) 0.93889(14) 0.0348(9) Uiso 1.000000 R
H25 H 0.3624(3) 0.9517(3) 0.86365(14) 0.0353(9) Uiso 1.000000 R
H26 H 0.4300(3) 0.8506(2) 0.80638(13) 0.0292(9) Uiso 1.000000 R
H22 H 0.7477(3) 0.8463(2) 0.90037(13) 0.0289(8) Uiso 1.000000 R
H17 H 0.4461(3) 0.6359(2) 0.84448(13) 0.0276(8) Uiso 1.000000 R
H16 H 0.4793(3) 0.5218(2) 0.90852(13) 0.0323(9) Uiso 1.000000 R
H15 H 0.6004(3) 0.3978(2) 0.89898(14) 0.0350(9) Uiso 1.000000 R
H14 H 0.6882(3) 0.3862(2) 0.82505(14) 0.0336(9) Uiso 1.000000 R
H13 H 0.6542(3) 0.4994(2) 0.76035(13) 0.0275(8) Uiso 1.000000 R
H5 H 0.6415(3) 0.8296(3) 0.55691(14) 0.0340(9) Uiso 1.000000 R
H4 H 0.5840(3) 0.8508(3) 0.46802(14) 0.0365(10) Uiso 1.000000 R
H3 H 0.4264(3) 0.7693(3) 0.42257(14) 0.0366(10) Uiso 1.000000 R
H2 H 0.3206(3) 0.6698(3) 0.46758(14) 0.0363(10) Uiso 1.000000 R
H1 H 0.3764(3) 0.6481(3) 0.55668(14) 0.0327(9) Uiso 1.000000 R
H50 H 1.0001(3) 0.4690(3) 0.94813(14) 0.0365(10) Uiso 1.000000 R
H51 H 0.8711(3) 0.5209(3) 0.87477(14) 0.0356(9) Uiso 1.000000 R
H52 H 0.9335(3) 0.6244(2) 0.81686(13) 0.0309(9) Uiso 1.000000 R
H48 H 1.2563(3) 0.6261(2) 0.90608(13) 0.0298(9) Uiso 1.000000 R
H43 H 0.9658(3) 0.8287(2) 0.86034(13) 0.0325(9) Uiso 1.000000 R
H42 H 0.9951(3) 0.9389(3) 0.92625(14) 0.0403(10) Uiso 1.000000 R
H41 H 1.0868(3) 1.0780(3) 0.91314(15) 0.0395(10) Uiso 1.000000 R
H40 H 1.1532(3) 1.1041(3) 0.83480(15) 0.0402(10) Uiso 1.000000 R
H39 H 1.1262(3) 0.9932(2) 0.76933(14) 0.0325(9) Uiso 1.000000 R
H31 H 1.1873(3) 0.7553(3) 0.55643(15) 0.0364(10) Uiso 1.000000 R
H30 H 1.1242(4) 0.7461(3) 0.46705(15) 0.0422(11) Uiso 1.000000 R
H29 H 0.9261(4) 0.7561(3) 0.43253(14) 0.0399(10) Uiso 1.000000 R
H28 H 0.7887(3) 0.7690(3) 0.48784(14) 0.0362(10) Uiso 1.000000 R
H27 H 0.8502(3) 0.7756(2) 0.57772(14) 0.0334(9) Uiso 1.000000 R
H9 H 0.6923(3) 0.6578(2) 0.73504(12) 0.0253(8) Uiso 1.000000 R
H10 H 0.5169(3) 0.7986(2) 0.74451(13) 0.0251(8) Uiso 1.000000 R
H19a H 0.2412(6) 0.5766(17) 0.6469(3) 0.0443(12) Uiso 1.000000 GR
H19b H 0.2139(10) 0.4912(4) 0.6804(8) 0.0443(12) Uiso 1.000000 GR
H19c H 0.1838(5) 0.5916(15) 0.6971(6) 0.0443(12) Uiso 1.000000 GR
H35 H 1.1931(3) 0.8253(2) 0.74818(13) 0.0280(8) Uiso 1.000000 R
H36 H 1.0183(3) 0.6825(2) 0.75284(13) 0.0270(8) Uiso 1.000000 R
H45a H 0.7505(7) 0.9121(17) 0.6579(3) 0.0466(12) Uiso 1.000000 GR
H45b H 0.6847(6) 0.8945(14) 0.7053(6) 0.0466(12) Uiso 1.000000 GR
H45c H 0.7209(12) 0.9955(4) 0.6924(8) 0.0466(12) Uiso 1.000000 GR


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C23 1.904(3) . ?
O1 C18 1.194(4) . ?
O2 C18 1.336(4) . ?
O2 C19 1.453(4) . ?
O3 C20 1.224(4) . ?
C1 C2 1.379(5) . ?
C1 C6 1.401(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.389(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.380(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.435(5) . ?
C7 C8 1.193(5) . ?
C8 C9 1.444(5) . ?
C9 C10 1.512(4) . ?
C9 C11 1.527(4) . ?
C9 H9 0.9800 . ?
C10 C11 1.535(4) . ?
C10 C20 1.494(4) . ?
C10 H10 0.9800 . ?
C11 C12 1.495(4) . ?
C11 C18 1.512(4) . ?
C12 C13 1.392(5) . ?
C12 C17 1.392(4) . ?
C13 C14 1.393(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.385(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.381(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.391(5) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C19 H19a 0.9600 . ?
C19 H19b 0.9600 . ?
C19 H19c 0.9600 . ?
C20 C21 1.496(5) . ?
C21 C22 1.396(5) . ?
C21 C26 1.400(5) . ?
C22 C23 1.380(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.387(5) . ?
C24 C25 1.375(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.383(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
Br2 C49 1.903(3) . ?
O4 C44 1.340(4) . ?
O4 C45 1.448(4) . ?
O5 C44 1.203(4) . ?
O6 C46 1.223(4) . ?
C27 C28 1.383(5) . ?
C27 C32 1.397(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.384(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.384(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.377(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.400(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.430(5) . ?
C33 C34 1.197(5) . ?
C34 C35 1.434(5) . ?
C35 C36 1.505(5) . ?
C35 C37 1.524(4) . ?
C35 H35 0.9800 . ?
C36 C37 1.517(5) . ?
C36 C46 1.495(5) . ?
C36 H36 0.9800 . ?
C37 C38 1.500(4) . ?
C37 C44 1.513(4) . ?
C38 C39 1.390(5) . ?
C38 C43 1.388(5) . ?
C39 C40 1.385(5) . ?
C39 H39 0.9300 . ?
C40 C41 1.383(6) . ?
C40 H40 0.9300 . ?
C41 C42 1.387(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.387(5) . ?
C42 H42 0.9300 . ?
C43 H43 0.9300 . ?
C45 H45a 0.9600 . ?
C45 H45b 0.9600 . ?
C45 H45c 0.9600 . ?
C46 C47 1.494(5) . ?
C47 C48 1.398(5) . ?
C47 C52 1.390(5) . ?
C48 C49 1.380(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.378(5) . ?
C50 C51 1.389(5) . ?
C50 H50 0.9300 . ?
C51 C52 1.389(5) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 O2 C18 114.8(3) . . ?
C6 C1 C2 120.5(3) . . ?
H1 C1 C2 119.7(2) . . ?
H1 C1 C6 119.7(2) . . ?
C3 C2 C1 120.3(3) . . ?
H2 C2 C1 119.8(2) . . ?
H2 C2 C3 119.8(2) . . ?
C4 C3 C2 119.5(3) . . ?
H3 C3 C2 120.2(2) . . ?
H3 C3 C4 120.2(2) . . ?
C5 C4 C3 120.6(3) . . ?
H4 C4 C3 119.7(2) . . ?
H4 C4 C5 119.7(2) . . ?
C6 C5 C4 120.6(3) . . ?
H5 C5 C4 119.7(2) . . ?
H5 C5 C6 119.7(2) . . ?
C5 C6 C1 118.4(3) . . ?
C7 C6 C1 120.0(3) . . ?
C7 C6 C5 121.7(3) . . ?
C8 C7 C6 178.7(4) . . ?
C9 C8 C7 177.0(3) . . ?
C10 C9 C8 119.1(3) . . ?
C11 C9 C8 120.0(3) . . ?
C11 C9 C10 60.7(2) . . ?
H9 C9 C8 115.39(18) . . ?
H9 C9 C10 115.39(17) . . ?
H9 C9 C11 115.39(17) . . ?
C11 C10 C9 60.2(2) . . ?
C20 C10 C9 119.6(3) . . ?
C20 C10 C11 118.4(3) . . ?
H10 C10 C9 115.76(17) . . ?
H10 C10 C11 115.76(17) . . ?
H10 C10 C20 115.76(18) . . ?
C10 C11 C9 59.2(2) . . ?
C12 C11 C9 120.4(3) . . ?
C12 C11 C10 121.1(3) . . ?
C18 C11 C9 114.7(3) . . ?
C18 C11 C10 112.3(3) . . ?
C18 C11 C12 116.7(3) . . ?
C13 C12 C11 121.2(3) . . ?
C17 C12 C11 119.6(3) . . ?
C17 C12 C13 119.2(3) . . ?
C14 C13 C12 120.3(3) . . ?
H13 C13 C12 119.83(19) . . ?
H13 C13 C14 119.8(2) . . ?
C15 C14 C13 119.9(3) . . ?
H14 C14 C13 120.1(2) . . ?
H14 C14 C15 120.1(2) . . ?
C16 C15 C14 120.1(3) . . ?
H15 C15 C14 119.9(2) . . ?
H15 C15 C16 119.9(2) . . ?
C17 C16 C15 120.2(3) . . ?
H16 C16 C15 119.9(2) . . ?
H16 C16 C17 119.9(2) . . ?
C16 C17 C12 120.2(3) . . ?
H17 C17 C12 119.90(19) . . ?
H17 C17 C16 119.9(2) . . ?
O2 C18 O1 123.7(3) . . ?
C11 C18 O1 125.0(3) . . ?
C11 C18 O2 111.2(3) . . ?
H19a C19 O2 109.5 . . ?
H19b C19 O2 109.5 . . ?
H19b C19 H19a 109.5 . . ?
H19c C19 O2 109.5 . . ?
H19c C19 H19a 109.5 . . ?
H19c C19 H19b 109.5 . . ?
C10 C20 O3 121.6(3) . . ?
C21 C20 O3 121.3(3) . . ?
C21 C20 C10 117.0(3) . . ?
C22 C21 C20 117.9(3) . . ?
C26 C21 C20 122.7(3) . . ?
C26 C21 C22 119.4(3) . . ?
C23 C22 C21 119.0(3) . . ?
H22 C22 C21 120.51(19) . . ?
H22 C22 C23 120.5(2) . . ?
C22 C23 Br1 118.6(3) . . ?
C24 C23 Br1 119.3(3) . . ?
C24 C23 C22 122.0(3) . . ?
C25 C24 C23 118.6(3) . . ?
H24 C24 C23 120.7(2) . . ?
H24 C24 C25 120.7(2) . . ?
C26 C25 C24 121.1(3) . . ?
H25 C25 C24 119.5(2) . . ?
H25 C25 C26 119.5(2) . . ?
C25 C26 C21 120.0(3) . . ?
H26 C26 C21 120.02(19) . . ?
H26 C26 C25 120.0(2) . . ?
C45 O4 C44 115.2(3) . . ?
C32 C27 C28 120.4(3) . . ?
H27 C27 C28 119.8(2) . . ?
H27 C27 C32 119.8(2) . . ?
C29 C28 C27 119.8(3) . . ?
H28 C28 C27 120.1(2) . . ?
H28 C28 C29 120.1(2) . . ?
C30 C29 C28 120.2(3) . . ?
H29 C29 C28 119.9(2) . . ?
H29 C29 C30 119.9(2) . . ?
C31 C30 C29 120.4(3) . . ?
H30 C30 C29 119.8(2) . . ?
H30 C30 C31 119.8(2) . . ?
C32 C31 C30 120.1(3) . . ?
H31 C31 C30 120.0(2) . . ?
H31 C31 C32 120.0(2) . . ?
C31 C32 C27 119.0(3) . . ?
C33 C32 C27 119.7(3) . . ?
C33 C32 C31 121.3(3) . . ?
C34 C33 C32 177.3(3) . . ?
C35 C34 C33 177.3(3) . . ?
C36 C35 C34 120.5(3) . . ?
C37 C35 C34 120.0(3) . . ?
C37 C35 C36 60.1(2) . . ?
H35 C35 C34 115.07(18) . . ?
H35 C35 C36 115.07(18) . . ?
H35 C35 C37 115.07(17) . . ?
C37 C36 C35 60.6(2) . . ?
C46 C36 C35 118.6(3) . . ?
C46 C36 C37 119.5(3) . . ?
H36 C36 C35 115.68(18) . . ?
H36 C36 C37 115.68(17) . . ?
H36 C36 C46 115.68(19) . . ?
C36 C37 C35 59.3(2) . . ?
C38 C37 C35 120.1(3) . . ?
C38 C37 C36 122.1(3) . . ?
C44 C37 C35 113.5(3) . . ?
C44 C37 C36 113.1(3) . . ?
C44 C37 C38 116.5(3) . . ?
C39 C38 C37 121.2(3) . . ?
C43 C38 C37 119.7(3) . . ?
C43 C38 C39 119.0(3) . . ?
C40 C39 C38 120.4(3) . . ?
H39 C39 C38 119.8(2) . . ?
H39 C39 C40 119.8(2) . . ?
C41 C40 C39 120.4(3) . . ?
H40 C40 C39 119.8(2) . . ?
H40 C40 C41 119.8(2) . . ?
C42 C41 C40 119.6(3) . . ?
H41 C41 C40 120.2(2) . . ?
H41 C41 C42 120.2(2) . . ?
C43 C42 C41 120.0(4) . . ?
H42 C42 C41 120.0(2) . . ?
H42 C42 C43 120.0(2) . . ?
C42 C43 C38 120.6(3) . . ?
H43 C43 C38 119.7(2) . . ?
H43 C43 C42 119.7(2) . . ?
O5 C44 O4 124.2(3) . . ?
C37 C44 O4 110.9(3) . . ?
C37 C44 O5 124.8(3) . . ?
H45a C45 O4 109.5 . . ?
H45b C45 O4 109.5 . . ?
H45b C45 H45a 109.5 . . ?
H45c C45 O4 109.5 . . ?
H45c C45 H45a 109.5 . . ?
H45c C45 H45b 109.5 . . ?
C36 C46 O6 120.9(3) . . ?
C47 C46 O6 121.0(3) . . ?
C47 C46 C36 118.2(3) . . ?
C48 C47 C46 117.4(3) . . ?
C52 C47 C46 122.9(3) . . ?
C52 C47 C48 119.6(3) . . ?
C49 C48 C47 119.3(3) . . ?
H48 C48 C47 120.4(2) . . ?
H48 C48 C49 120.4(2) . . ?
C48 C49 Br2 118.1(3) . . ?
C50 C49 Br2 119.9(3) . . ?
C50 C49 C48 121.9(3) . . ?
C51 C50 C49 118.4(3) . . ?
H50 C50 C49 120.8(2) . . ?
H50 C50 C51 120.8(2) . . ?
C52 C51 C50 121.0(3) . . ?
H51 C51 C50 119.5(2) . . ?
H51 C51 C52 119.5(2) . . ?
C51 C52 C47 119.8(3) . . ?
H52 C52 C47 120.1(2) . . ?
H52 C52 C51 120.1(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.252
_oxdiff_exptl_absorpt_empirical_full_min 0.465
####################################################################### 
# 
# 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_exp_1907
_database_code_depnum_ccdc_archive 'CCDC 2180630'
loop_
_audit_author_name
_audit_author_address
'Sunewang Rixin Wang'
;East China Normal University
China
;
_audit_update_record             
;
2022-06-21 deposited with the CCDC.	2022-10-02 downloaded from the CCDC.
;
_audit_creation_date             2021-04-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H19 Br O3'
_chemical_formula_sum            'C26 H19 Br O3'
_chemical_formula_weight         459.32
_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'
Br Br -0.6763 1.2805 '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                   15.2783(2)
_cell_length_b                   10.33270(10)
_cell_length_c                   15.5266(2)
_cell_angle_alpha                90
_cell_angle_beta                 118.164(2)
_cell_angle_gamma                90
_cell_volume                     2160.91(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16408
_cell_measurement_temperature    170(1)
_cell_measurement_theta_max      74.1870
_cell_measurement_theta_min      3.2880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.788
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21837
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         5.364
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  18.00   1.00    1.00    --    0.00 -38.00  90.00   53
  2  ω    -88.00  -5.00   1.00    1.00    --    0.00 -77.00 -90.00   83
  3  ω    -14.00  12.00   1.00    1.00    --    0.00  38.00 -60.00   26
  4  ω     32.00  85.00   1.00    1.00    --    0.00  38.00   0.00   53
  5  ω    -83.00 -56.00   1.00    1.00    --    0.00 -38.00  90.00   27
  6  ω    -74.00  15.00   1.00    1.00    --    0.00 -38.00   0.00   89
  7  ω     10.00 127.00   1.00    1.00    --   95.80 -82.00 -90.00  117
  8  ω     26.00  81.00   1.00    1.00    --   95.80 -61.00 -90.00   55
  9  ω     76.00 140.00   1.00    1.00    --   95.80  30.00  30.00   64
 10  ω     88.00 128.00   1.00    1.00    --   95.80 -82.00-150.00   40
 11  ω     45.00  71.00   1.00    1.00    --   95.80 -82.00-150.00   26
 12  ω     88.00 114.00   1.00    1.00    --   95.80 -61.00 -90.00   26
 13  ω     79.00 128.00   1.00    1.00    --   95.80 -82.00 150.00   49
 14  ω     16.00 119.00   1.00    1.00    --   95.80 -61.00  60.00  103
 15  ω     20.00  45.00   1.00    1.00    --   95.80 -82.00   0.00   25
 16  ω    118.00 184.00   1.00    1.00    --   95.80  15.00-150.00   66
 17  ω     70.00 101.00   1.00    1.00    --   95.80  15.00-150.00   31
 18  ω     53.00  78.00   1.00    1.00    --   95.80 -82.00   0.00   25
 19  ω     79.00 105.00   1.00    1.00    --   95.80 -82.00   0.00   26
 20  ω     85.00 128.00   1.00    1.00    --   95.80 -82.00 120.00   43
 21  ω     78.00 103.00   1.00    1.00    --   95.80  30.00 -90.00   25
 22  ω    124.00 185.00   1.00    1.00    --   95.80  30.00 -90.00   61
 23  ω     63.00 115.00   1.00    1.00    --   95.80 -30.00  90.00   52
 24  ω    157.00 185.00   1.00    1.00    --   95.80  30.00  30.00   28
 25  ω     71.00  96.00   1.00    1.00    --   95.80 -82.00 -60.00   25
 26  ω     78.00 103.00   1.00    1.00    --   95.80 -82.00 -30.00   25
 27  ω      9.00 122.00   1.00    1.00    --   95.80 -82.00  60.00  113
 28  ω     73.00 185.00   1.00    1.00    --   95.80  15.00 -30.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1102801000
_diffrn_orient_matrix_UB_12      -0.0356371000
_diffrn_orient_matrix_UB_13      0.0626134000
_diffrn_orient_matrix_UB_21      0.0299781000
_diffrn_orient_matrix_UB_22      0.1382653000
_diffrn_orient_matrix_UB_23      -0.0125862000
_diffrn_orient_matrix_UB_31      -0.0049114000
_diffrn_orient_matrix_UB_32      0.0428921000
_diffrn_orient_matrix_UB_33      0.0926461000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3680
_reflns_number_total             3851
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.078
_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)+(0.0484P)²+1.0306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0887
_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 Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C16(H16), C22(H22), C26(H26), C25(H25), C23(H23), C15(H15),
 C1(H1), C9(H9), C11(H11), C10(H10), C5(H5), C2(H2), C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.60260(2) 0.21720(3) 0.61512(2) 0.05044(11) Uani 1 1 d . . . . .
O1 O 0.16815(10) 0.27349(11) 0.17070(11) 0.0345(3) Uani 1 1 d . . . . .
O3 O 0.35996(11) 0.15373(14) 0.12541(11) 0.0450(4) Uani 1 1 d . . . . .
O2 O 0.24606(11) 0.29035(13) 0.02077(10) 0.0416(3) Uani 1 1 d . . . . .
C7 C 0.12543(13) 0.46765(16) 0.22201(12) 0.0251(3) Uani 1 1 d . . . . .
C13 C 0.26012(12) 0.45217(16) 0.16704(12) 0.0247(3) Uani 1 1 d . . . . .
C18 C 0.18306(12) 0.39068(16) 0.18479(12) 0.0247(3) Uani 1 1 d . . . . .
C17 C 0.34915(13) 0.37085(17) 0.17971(14) 0.0288(4) Uani 1 1 d . . . . .
C21 C 0.41093(12) 0.32943(17) 0.28646(13) 0.0278(4) Uani 1 1 d . . . . .
C14 C 0.26709(13) 0.57262(17) 0.13582(13) 0.0277(4) Uani 1 1 d . . . . .
C8 C 0.02566(14) 0.43760(18) 0.18945(15) 0.0328(4) Uani 1 1 d . . . . .
H8 H -0.004033 0.371054 0.144623 0.039 Uiso 1 1 calc R . . . .
C12 C 0.16949(15) 0.56550(17) 0.29017(13) 0.0318(4) Uani 1 1 d . . . . .
H12 H 0.235854 0.586435 0.312086 0.038 Uiso 1 1 calc R . . . .
C24 C 0.52151(14) 0.26512(19) 0.48254(14) 0.0326(4) Uani 1 1 d . . . . .
C6 C 0.20037(15) 0.68508(17) 0.11319(13) 0.0298(4) Uani 1 1 d . . . . .
C16 C 0.40419(14) 0.4664(2) 0.14867(15) 0.0360(4) Uani 1 1 d . . . . .
H16 H 0.462769 0.448480 0.146509 0.043 Uiso 1 1 calc R . . . .
C22 C 0.48787(14) 0.40906(17) 0.35078(14) 0.0323(4) Uani 1 1 d . . . . .
H22 H 0.502189 0.484762 0.327504 0.039 Uiso 1 1 calc R . . . .
C26 C 0.38964(13) 0.21771(17) 0.32353(14) 0.0308(4) Uani 1 1 d . . . . .
H26 H 0.337879 0.164285 0.281962 0.037 Uiso 1 1 calc R . . . .
C25 C 0.44445(14) 0.18510(18) 0.42138(14) 0.0324(4) Uani 1 1 d . . . . .
H25 H 0.429672 0.110575 0.445558 0.039 Uiso 1 1 calc R . . . .
C19 C 0.31915(14) 0.25692(18) 0.10769(14) 0.0322(4) Uani 1 1 d . . . . .
C23 C 0.54312(14) 0.37748(18) 0.44837(15) 0.0352(4) Uani 1 1 d . . . . .
H23 H 0.594250 0.431272 0.490526 0.042 Uiso 1 1 calc R . . . .
C15 C 0.35725(15) 0.57909(19) 0.12502(15) 0.0362(4) Uani 1 1 d . . . . .
H15 H 0.378420 0.651662 0.104563 0.043 Uiso 1 1 calc R . . . .
C1 C 0.09801(16) 0.6723(2) 0.06787(14) 0.0392(4) Uani 1 1 d . . . . .
H1 H 0.069009 0.591612 0.046015 0.047 Uiso 1 1 calc R . . . .
C9 C -0.02892(17) 0.5064(2) 0.22359(19) 0.0468(5) Uani 1 1 d . . . . .
H9 H -0.095775 0.487358 0.200568 0.056 Uiso 1 1 calc R . . . .
C11 C 0.11418(19) 0.63219(19) 0.32564(17) 0.0451(5) Uani 1 1 d . . . . .
H11 H 0.143978 0.696598 0.372381 0.054 Uiso 1 1 calc R . . . .
C10 C 0.01503(19) 0.6030(2) 0.2916(2) 0.0520(6) Uani 1 1 d . . . . .
H10 H -0.022058 0.648777 0.314718 0.062 Uiso 1 1 calc R . . . .
C5 C 0.2415(2) 0.80900(19) 0.13932(16) 0.0476(6) Uani 1 1 d . . . . .
H5 H 0.309674 0.820264 0.165133 0.057 Uiso 1 1 calc R . . . .
C20 C 0.21737(18) 0.1929(2) -0.05485(17) 0.0486(5) Uani 1 1 d . . . . .
H20A H 0.164363 0.225600 -0.114612 0.073 Uiso 1 1 calc GR . . . .
H20B H 0.195487 0.116523 -0.035379 0.073 Uiso 1 1 calc GR . . . .
H20C H 0.273254 0.172035 -0.064669 0.073 Uiso 1 1 calc GR . . . .
C2 C 0.0385(2) 0.7803(3) 0.05503(19) 0.0663(9) Uani 1 1 d . . . . .
H2 H -0.030153 0.771718 0.025130 0.080 Uiso 1 1 calc R . . . .
C4 C 0.1815(3) 0.9143(2) 0.12698(19) 0.0737(10) Uani 1 1 d . . . . .
H4 H 0.209641 0.995964 0.146411 0.088 Uiso 1 1 calc R . . . .
C3 C 0.0817(3) 0.9001(3) 0.0868(2) 0.0837(12) Uani 1 1 d . . . . .
H3 H 0.042138 0.971530 0.080509 0.100 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C24 1.900(2) . ?
O1 C18 1.232(2) . ?
O3 C19 1.200(2) . ?
O2 C19 1.329(2) . ?
O2 C20 1.449(2) . ?
C7 C18 1.491(2) . ?
C7 C8 1.396(2) . ?
C7 C12 1.387(3) . ?
C13 C18 1.474(2) . ?
C13 C17 1.530(2) . ?
C13 C14 1.358(2) . ?
C17 C21 1.531(3) . ?
C17 C16 1.516(2) . ?
C17 C19 1.537(2) . ?
C21 C22 1.396(3) . ?
C21 C26 1.395(3) . ?
C14 C6 1.475(2) . ?
C14 C15 1.466(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.378(3) . ?
C12 H12 0.9300 . ?
C12 C11 1.390(3) . ?
C24 C25 1.384(3) . ?
C24 C23 1.380(3) . ?
C6 C1 1.385(3) . ?
C6 C5 1.399(3) . ?
C16 H16 0.9300 . ?
C16 C15 1.325(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.381(3) . ?
C26 H26 0.9300 . ?
C26 C25 1.386(3) . ?
C25 H25 0.9300 . ?
C23 H23 0.9300 . ?
C15 H15 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.393(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.377(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.382(3) . ?
C10 H10 0.9300 . ?
C5 H5 0.9300 . ?
C5 C4 1.377(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C2 H2 0.9300 . ?
C2 C3 1.379(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.355(5) . ?
C3 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 O2 C20 115.49(16) . . ?
C8 C7 C18 119.00(16) . . ?
C12 C7 C18 121.47(15) . . ?
C12 C7 C8 119.50(16) . . ?
C18 C13 C17 118.64(14) . . ?
C14 C13 C18 131.76(16) . . ?
C14 C13 C17 109.53(15) . . ?
O1 C18 C7 119.97(15) . . ?
O1 C18 C13 119.17(15) . . ?
C13 C18 C7 120.84(14) . . ?
C13 C17 C21 110.43(14) . . ?
C13 C17 C19 112.65(15) . . ?
C21 C17 C19 113.15(15) . . ?
C16 C17 C13 101.20(14) . . ?
C16 C17 C21 112.05(15) . . ?
C16 C17 C19 106.70(15) . . ?
C22 C21 C17 119.37(16) . . ?
C26 C21 C17 122.23(16) . . ?
C26 C21 C22 118.31(17) . . ?
C13 C14 C6 130.19(16) . . ?
C13 C14 C15 108.60(16) . . ?
C15 C14 C6 121.21(16) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.12(19) . . ?
C9 C8 H8 119.9 . . ?
C7 C12 H12 120.1 . . ?
C7 C12 C11 119.80(18) . . ?
C11 C12 H12 120.1 . . ?
C25 C24 Br1 119.75(15) . . ?
C23 C24 Br1 118.93(14) . . ?
C23 C24 C25 121.28(19) . . ?
C1 C6 C14 122.25(17) . . ?
C1 C6 C5 118.63(19) . . ?
C5 C6 C14 119.11(19) . . ?
C17 C16 H16 124.7 . . ?
C15 C16 C17 110.58(16) . . ?
C15 C16 H16 124.7 . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.19(17) . . ?
C23 C22 H22 119.4 . . ?
C21 C26 H26 119.5 . . ?
C25 C26 C21 121.02(17) . . ?
C25 C26 H26 119.5 . . ?
C24 C25 C26 119.00(18) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
O3 C19 O2 124.10(18) . . ?
O3 C19 C17 124.72(18) . . ?
O2 C19 C17 111.04(15) . . ?
C24 C23 C22 119.17(17) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C14 C15 H15 125.0 . . ?
C16 C15 C14 110.08(17) . . ?
C16 C15 H15 125.0 . . ?
C6 C1 H1 120.0 . . ?
C6 C1 C2 120.0(2) . . ?
C2 C1 H1 120.0 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.3(2) . . ?
C10 C9 H9 119.8 . . ?
C12 C11 H11 119.9 . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C9 C10 C11 120.08(19) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C6 C5 H5 119.9 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.9 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 H2 120.1 . . ?
C5 C4 H4 119.7 . . ?
C3 C4 C5 120.6(3) . . ?
C3 C4 H4 119.7 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.776
_oxdiff_exptl_absorpt_empirical_full_min 0.700
####################################################################### 
# 
# 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_exp_2452
_database_code_depnum_ccdc_archive 'CCDC 2180631'
loop_
_audit_author_name
_audit_author_address
'Sunewang Rixin Wang'
;East China Normal University
China
;
_audit_update_record             
;
2022-06-21 deposited with the CCDC.	2022-10-02 downloaded from the CCDC.
;
_audit_creation_date             2021-12-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H25 N O3'
_chemical_formula_sum            'C33 H25 N O3'
_chemical_formula_weight         483.54
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.1720(3)
_cell_length_b                   10.8609(4)
_cell_length_c                   11.9780(4)
_cell_angle_alpha                91.906(3)
_cell_angle_beta                 103.416(3)
_cell_angle_gamma                102.090(3)
_cell_volume                     1253.96(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8036
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.9790
_cell_measurement_theta_min      4.5730
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.819
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11615
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.808
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     38.00  86.00   1.00    1.00    --    0.00  37.00  60.00   48
  2  ω     29.00  56.00   1.00    1.00    --    0.00  37.00-180.00   27
  3  ω     -6.00  19.00   1.00    1.00    --    0.00 -37.00  90.00   25
  4  ω    -84.00 -35.00   1.00    1.00    --    0.00 -57.00-180.00   49
  5  ω    -27.00  19.00   1.00    1.00    --    0.00 -57.00-180.00   46
  6  ω    -17.00  21.00   1.00    1.00    --    0.00  37.00  60.00   38
  7  ω    -88.00 -27.00   1.00    1.00    --    0.00 -37.00  90.00   61
  8  ω     30.00 128.00   1.00    1.00    --   95.80 -82.00 -90.00   98
  9  ω     72.00 160.00   1.00    1.00    --   95.80  61.00  30.00   88
 10  ω     10.00 122.00   1.00    1.00    --   95.80 -82.00-180.00  112
 11  ω      6.00 110.00   1.00    1.00    --   95.80 -61.00-180.00  104
 12  ω     78.00 103.00   1.00    1.00    --   95.80 -82.00 -30.00   25
 13  ω     79.00 117.00   1.00    1.00    --   95.80 -61.00-120.00   38
 14  ω     34.00  77.00   1.00    1.00    --   95.80 -77.00 -30.00   43
 15  ω     16.00  46.00   1.00    1.00    --   95.80 -61.00-120.00   30
 16  ω     21.00 117.00   1.00    1.00    --   95.80 -82.00  60.00   96
 17  ω     18.00 101.00   1.00    1.00    --   95.80 -61.00  60.00   83
 18  ω    152.00 178.00   1.00    1.00    --   95.80  30.00 -60.00   26
 19  ω     88.00 179.00   1.00    1.00    --   95.80  45.00 120.00   91
 20  ω     86.00 154.00   1.00    1.00    --   95.80  82.00   0.00   68
 21  ω     77.00 102.00   1.00    1.00    --   95.80 -82.00  90.00   25
 22  ω    116.00 174.00   1.00    1.00    --   95.80  45.00  90.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0197009000
_diffrn_orient_matrix_UB_12      0.1356547000
_diffrn_orient_matrix_UB_13      -0.0373912000
_diffrn_orient_matrix_UB_21      -0.0486683000
_diffrn_orient_matrix_UB_22      -0.0528940000
_diffrn_orient_matrix_UB_23      -0.1273270000
_diffrn_orient_matrix_UB_31      -0.1508605000
_diffrn_orient_matrix_UB_32      0.0003411000
_diffrn_orient_matrix_UB_33      0.0018286000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4079
_reflns_number_total             4436
_reflns_odcompleteness_completeness 99.60
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0133(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.061
_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)+(0.0431P)²+0.2578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0900
_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.a Ternary CH refined with riding coordinates:
 C8(H8), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C13(H13), C14(H14), C15(H15),
 C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29),
  C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.54682(9) 0.16621(8) 0.12338(7) 0.0357(2) Uani 1 1 d . . . . .
O3 O 0.94893(9) 1.16795(8) 0.09257(8) 0.0365(2) Uani 1 1 d . . . . .
O2 O 0.67108(8) 0.57254(8) 0.42595(7) 0.0320(2) Uani 1 1 d . . . . .
N1 N 0.82263(9) 0.45826(8) 0.52285(8) 0.0241(2) Uani 1 1 d . . . . .
C1 C 0.41651(13) 0.20381(12) 0.37709(11) 0.0356(3) Uani 1 1 d . . . . .
H1 H 0.441375 0.291409 0.390413 0.043 Uiso 1 1 calc R . . . .
C2 C 0.35019(15) 0.13256(14) 0.45003(13) 0.0445(3) Uani 1 1 d . . . . .
H2 H 0.330128 0.172274 0.512028 0.053 Uiso 1 1 calc R . . . .
C3 C 0.31386(14) 0.00242(14) 0.43060(14) 0.0470(4) Uani 1 1 d . . . . .
H3 H 0.270281 -0.045326 0.480207 0.056 Uiso 1 1 calc R . . . .
C4 C 0.34184(14) -0.05731(13) 0.33791(14) 0.0444(3) Uani 1 1 d . . . . .
H4 H 0.316531 -0.144933 0.324999 0.053 Uiso 1 1 calc R . . . .
C5 C 0.40741(13) 0.01316(12) 0.26447(12) 0.0362(3) Uani 1 1 d . . . . .
H5 H 0.425827 -0.027146 0.201971 0.043 Uiso 1 1 calc R . . . .
C6 C 0.44612(11) 0.14461(11) 0.28371(10) 0.0292(3) Uani 1 1 d . . . . .
C7 C 0.52388(11) 0.21697(11) 0.20686(10) 0.0273(3) Uani 1 1 d . . . . .
C8 C 0.58236(11) 0.35551(11) 0.24160(9) 0.0264(2) Uani 1 1 d . . . . .
H8 H 0.515031 0.406530 0.247593 0.032 Uiso 1 1 calc R . . . .
C9 C 0.70879(12) 0.42137(11) 0.20648(9) 0.0270(3) Uani 1 1 d . . . . .
H9 H 0.746171 0.366391 0.161477 0.032 Uiso 1 1 calc R . . . .
C10 C 0.71900(11) 0.38851(10) 0.33270(9) 0.0238(2) Uani 1 1 d . . . . .
C11 C 0.73197(11) 0.48672(10) 0.42851(9) 0.0239(2) Uani 1 1 d . . . . .
C12 C 0.87012(11) 0.35042(10) 0.49760(9) 0.0233(2) Uani 1 1 d . . . . .
C13 C 0.97034(12) 0.29963(11) 0.56726(10) 0.0279(3) Uani 1 1 d . . . . .
H13 H 1.012165 0.333176 0.642693 0.033 Uiso 1 1 calc R . . . .
C14 C 1.00623(12) 0.19609(11) 0.51993(11) 0.0319(3) Uani 1 1 d . . . . .
H14 H 1.073616 0.160046 0.564537 0.038 Uiso 1 1 calc R . . . .
C15 C 0.94337(13) 0.14589(11) 0.40764(11) 0.0319(3) Uani 1 1 d . . . . .
H15 H 0.968595 0.076436 0.378176 0.038 Uiso 1 1 calc R . . . .
C16 C 0.84264(12) 0.19846(11) 0.33835(10) 0.0277(3) Uani 1 1 d . . . . .
H16 H 0.800677 0.164805 0.262973 0.033 Uiso 1 1 calc R . . . .
C17 C 0.80642(11) 0.30138(10) 0.38379(9) 0.0232(2) Uani 1 1 d . . . . .
C18 C 0.85939(12) 0.52822(11) 0.63566(10) 0.0282(3) Uani 1 1 d . . . . .
H18A H 0.831077 0.608037 0.627634 0.034 Uiso 1 1 calc R . . . .
H18B H 0.959332 0.546749 0.664862 0.034 Uiso 1 1 calc R . . . .
C19 C 0.79248(11) 0.45662(10) 0.72181(9) 0.0245(2) Uani 1 1 d . . . . .
C20 C 0.87240(12) 0.43002(11) 0.82494(10) 0.0300(3) Uani 1 1 d . . . . .
H20 H 0.968534 0.454843 0.840813 0.036 Uiso 1 1 calc R . . . .
C21 C 0.81011(14) 0.36669(12) 0.90458(11) 0.0370(3) Uani 1 1 d . . . . .
H21 H 0.864483 0.349149 0.973411 0.044 Uiso 1 1 calc R . . . .
C22 C 0.66768(14) 0.32979(13) 0.88169(11) 0.0389(3) Uani 1 1 d . . . . .
H22 H 0.625900 0.287740 0.935214 0.047 Uiso 1 1 calc R . . . .
C23 C 0.58676(13) 0.35543(13) 0.77877(11) 0.0373(3) Uani 1 1 d . . . . .
H23 H 0.490654 0.330510 0.763170 0.045 Uiso 1 1 calc R . . . .
C24 C 0.64922(12) 0.41819(11) 0.69923(10) 0.0300(3) Uani 1 1 d . . . . .
H24 H 0.594653 0.434719 0.630062 0.036 Uiso 1 1 calc R . . . .
C25 C 0.73432(12) 0.55129(12) 0.18006(10) 0.0295(3) Uani 1 1 d . . . . .
C26 C 0.76745(12) 0.65970(11) 0.16099(10) 0.0297(3) Uani 1 1 d . . . . .
C27 C 0.81437(12) 0.78989(11) 0.14290(10) 0.0282(3) Uani 1 1 d . . . . .
C28 C 0.72146(13) 0.86488(12) 0.09721(10) 0.0319(3) Uani 1 1 d . . . . .
H28 H 0.626594 0.830216 0.078426 0.038 Uiso 1 1 calc R . . . .
C29 C 0.76939(13) 0.98947(12) 0.07989(10) 0.0327(3) Uani 1 1 d . . . . .
H29 H 0.706861 1.037880 0.048452 0.039 Uiso 1 1 calc R . . . .
C30 C 0.91108(13) 1.04311(11) 0.10930(10) 0.0286(3) Uani 1 1 d . . . . .
C31 C 1.00472(12) 0.97006(11) 0.15415(10) 0.0289(3) Uani 1 1 d . . . . .
H31 H 1.099498 1.005125 0.173209 0.035 Uiso 1 1 calc R . . . .
C32 C 0.95585(12) 0.84496(11) 0.17018(10) 0.0289(3) Uani 1 1 d . . . . .
H32 H 1.018838 0.796308 0.199895 0.035 Uiso 1 1 calc R . . . .
C33 C 1.09366(15) 1.22498(12) 0.12607(12) 0.0407(3) Uani 1 1 d . . . . .
H33A H 1.142495 1.180312 0.085074 0.061 Uiso 1 1 calc GR . . . .
H33B H 1.127532 1.221402 0.207398 0.061 Uiso 1 1 calc GR . . . .
H33C H 1.108237 1.311574 0.108255 0.061 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.2181(14) . ?
O3 C30 1.3645(14) . ?
O3 C33 1.4281(16) . ?
O2 C11 1.2201(13) . ?
N1 C11 1.3718(14) . ?
N1 C12 1.4064(14) . ?
N1 C18 1.4564(14) . ?
C1 H1 0.9300 . ?
C1 C2 1.3845(18) . ?
C1 C6 1.3947(18) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.382(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.3812(19) . ?
C5 H5 0.9300 . ?
C5 C6 1.3953(17) . ?
C6 C7 1.4887(16) . ?
C7 C8 1.5032(16) . ?
C8 H8 0.9800 . ?
C8 C9 1.4928(16) . ?
C8 C10 1.5207(15) . ?
C9 H9 0.9800 . ?
C9 C10 1.5500(15) . ?
C9 C25 1.4397(16) . ?
C10 C11 1.5038(15) . ?
C10 C17 1.4830(15) . ?
C12 C13 1.3824(16) . ?
C12 C17 1.3997(16) . ?
C13 H13 0.9300 . ?
C13 C14 1.3946(17) . ?
C14 H14 0.9300 . ?
C14 C15 1.3860(18) . ?
C15 H15 0.9300 . ?
C15 C16 1.3952(17) . ?
C16 H16 0.9300 . ?
C16 C17 1.3808(16) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.5134(15) . ?
C19 C20 1.3880(16) . ?
C19 C24 1.3877(16) . ?
C20 H20 0.9300 . ?
C20 C21 1.3878(17) . ?
C21 H21 0.9300 . ?
C21 C22 1.3784(19) . ?
C22 H22 0.9300 . ?
C22 C23 1.3866(19) . ?
C23 H23 0.9300 . ?
C23 C24 1.3852(17) . ?
C24 H24 0.9300 . ?
C25 C26 1.1999(17) . ?
C26 C27 1.4352(16) . ?
C27 C28 1.4029(16) . ?
C27 C32 1.3942(17) . ?
C28 H28 0.9300 . ?
C28 C29 1.3787(17) . ?
C29 H29 0.9300 . ?
C29 C30 1.3928(18) . ?
C30 C31 1.3902(16) . ?
C31 H31 0.9300 . ?
C31 C32 1.3816(16) . ?
C32 H32 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C30 O3 C33 116.74(9) . . ?
C11 N1 C12 111.34(9) . . ?
C11 N1 C18 123.84(9) . . ?
C12 N1 C18 124.77(9) . . ?
C2 C1 H1 119.9 . . ?
C2 C1 C6 120.20(12) . . ?
C6 C1 H1 119.9 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 119.91(13) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.44(12) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 119.98(13) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.25(13) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 119.22(11) . . ?
C1 C6 C7 121.95(11) . . ?
C5 C6 C7 118.76(11) . . ?
O1 C7 C6 122.24(11) . . ?
O1 C7 C8 120.84(10) . . ?
C6 C7 C8 116.79(10) . . ?
C7 C8 H8 116.1 . . ?
C7 C8 C10 115.75(9) . . ?
C9 C8 C7 119.85(10) . . ?
C9 C8 H8 116.1 . . ?
C9 C8 C10 61.90(7) . . ?
C10 C8 H8 116.1 . . ?
C8 C9 H9 114.0 . . ?
C8 C9 C10 59.93(7) . . ?
C10 C9 H9 114.0 . . ?
C25 C9 C8 124.08(10) . . ?
C25 C9 H9 114.0 . . ?
C25 C9 C10 120.25(10) . . ?
C8 C10 C9 58.16(7) . . ?
C11 C10 C8 117.10(9) . . ?
C11 C10 C9 122.17(9) . . ?
C17 C10 C8 127.66(10) . . ?
C17 C10 C9 120.61(9) . . ?
C17 C10 C11 105.70(9) . . ?
O2 C11 N1 125.86(10) . . ?
O2 C11 C10 127.67(10) . . ?
N1 C11 C10 106.42(9) . . ?
C13 C12 N1 128.00(10) . . ?
C13 C12 C17 122.08(10) . . ?
C17 C12 N1 109.80(9) . . ?
C12 C13 H13 121.3 . . ?
C12 C13 C14 117.36(11) . . ?
C14 C13 H13 121.3 . . ?
C13 C14 H14 119.4 . . ?
C15 C14 C13 121.24(11) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.70(11) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 H16 120.6 . . ?
C17 C16 C15 118.76(11) . . ?
C17 C16 H16 120.6 . . ?
C12 C17 C10 106.64(9) . . ?
C16 C17 C10 133.11(10) . . ?
C16 C17 C12 119.86(10) . . ?
N1 C18 H18A 109.1 . . ?
N1 C18 H18B 109.1 . . ?
N1 C18 C19 112.71(9) . . ?
H18A C18 H18B 107.8 . . ?
C19 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C20 C19 C18 120.93(10) . . ?
C24 C19 C18 120.12(10) . . ?
C24 C19 C20 118.94(10) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.58(11) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.02(12) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 120.0 . . ?
C21 C22 C23 119.94(11) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 119.93(12) . . ?
C24 C23 H23 120.0 . . ?
C19 C24 H24 119.7 . . ?
C23 C24 C19 120.59(11) . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C9 174.40(12) . . ?
C25 C26 C27 176.76(13) . . ?
C28 C27 C26 121.85(11) . . ?
C32 C27 C26 120.01(10) . . ?
C32 C27 C28 118.14(11) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 C27 120.65(11) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.26(11) . . ?
C30 C29 H29 119.9 . . ?
O3 C30 C29 116.28(10) . . ?
O3 C30 C31 123.84(11) . . ?
C31 C30 C29 119.88(11) . . ?
C30 C31 H31 120.3 . . ?
C32 C31 C30 119.47(11) . . ?
C32 C31 H31 120.3 . . ?
C27 C32 H32 119.2 . . ?
C31 C32 C27 121.59(10) . . ?
C31 C32 H32 119.2 . . ?
O3 C33 H33A 109.5 . . ?
O3 C33 H33B 109.5 . . ?
O3 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.455
_oxdiff_exptl_absorpt_empirical_full_min 0.552
####################################################################### 
# 
# 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_exp_2195
_database_code_depnum_ccdc_archive 'CCDC 2180632'
loop_
_audit_author_name
_audit_author_address
'Sunewang Rixin Wang'
;East China Normal University
China
;
_audit_update_record             
;
2022-06-21 deposited with the CCDC.	2022-10-02 downloaded from the CCDC.
;
_audit_creation_date             2021-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H22 Br N O2'
_chemical_formula_sum            'C32 H22 Br N O2'
_chemical_formula_weight         532.41
_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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   9.2610(4)
_cell_length_b                   11.3469(6)
_cell_length_c                   12.8776(7)
_cell_angle_alpha                85.549(4)
_cell_angle_beta                 74.375(5)
_cell_angle_gamma                76.275(4)
_cell_volume                     1265.87(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10931
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      74.1700
_cell_measurement_theta_min      5.0760
_shelx_estimated_absorpt_T_max   0.592
_shelx_estimated_absorpt_T_min   0.457
_exptl_absorpt_coefficient_mu    2.445
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12731
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.564
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_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    -44.00   4.00   1.00    1.00    --    0.00 -59.00  23.00   48
  2  ω     20.00  61.00   1.00    1.00    --    0.00  59.00 163.00   41
  3  ω    106.00 132.00   1.00    1.00    --   95.80  59.00 163.00   26
  4  ω     25.00 114.00   1.00    1.00    --   95.80 -59.00  23.00   89
  5  ω    -22.00  13.00   1.00    1.00    --    0.00  19.00 -30.00   35
  6  ω     14.00  88.00   1.00    1.00    --    0.00  38.00 -30.00   74
  7  ω     48.00  89.00   1.00    1.00    --    0.00  82.00  90.00   41
  8  ω    -29.00  42.00   1.00    1.00    --    0.00  82.00  90.00   71
  9  ω     68.00 150.00   1.00    1.00    --   95.80  15.00 -30.00   82
 10  ω      8.00  43.00   1.00    1.00    --   95.80 -82.00 120.00   35
 11  ω     57.00 114.00   1.00    1.00    --   95.80 -30.00-150.00   57
 12  ω     30.00  69.00   1.00    1.00    --   95.80 -82.00   0.00   39
 13  ω     44.00 128.00   1.00    1.00    --   95.80 -82.00-150.00   84
 14  ω     82.00 118.00   1.00    1.00    --   95.80 -82.00   0.00   36
 15  ω      6.00 116.00   1.00    1.00    --   95.80 -15.00 -60.00  110
 16  ω     13.00 120.00   1.00    1.00    --   95.80 -61.00  90.00  107
 17  ω     69.00 181.00   1.00    1.00    --   95.80  15.00-150.00  112
 18  ω     64.00 125.00   1.00    1.00    --   95.80 -77.00 -90.00   61
 19  ω     12.00  46.00   1.00    1.00    --   95.80 -77.00 -90.00   34
 20  ω     62.00 105.00   1.00    1.00    --   95.80 -82.00 120.00   43
 21  ω     45.00  75.00   1.00    1.00    --   95.80 -82.00  30.00   30
 22  ω     93.00 119.00   1.00    1.00    --   95.80 -82.00 -90.00   26
 23  ω      6.00  41.00   1.00    1.00    --   95.80 -30.00-150.00   35
 24  ω     81.00 106.00   1.00    1.00    --   95.80 -82.00  60.00   25
 25  ω     15.00 100.00   1.00    1.00    --   95.80 -61.00-150.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1566714000
_diffrn_orient_matrix_UB_12      0.0202463000
_diffrn_orient_matrix_UB_13      0.0050344000
_diffrn_orient_matrix_UB_21      -0.0085889000
_diffrn_orient_matrix_UB_22      0.0998540000
_diffrn_orient_matrix_UB_23      -0.0877385000
_diffrn_orient_matrix_UB_31      -0.0825201000
_diffrn_orient_matrix_UB_32      0.0956907000
_diffrn_orient_matrix_UB_33      0.0878145000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4324
_reflns_number_total             4506
_reflns_odcompleteness_completeness 99.67
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.040
_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)+(0.0421P)²+0.8724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0831
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.14442(2) 0.33972(2) 0.98543(2) 0.03270(9) Uani 1 1 d . . . . .
O1 O 0.92079(16) 0.47702(13) 0.73151(11) 0.0280(3) Uani 1 1 d . . . . .
O2 O 0.58224(19) 0.69748(13) 0.84606(11) 0.0329(3) Uani 1 1 d . . . . .
N1 N 0.70835(18) 0.41304(13) 0.83441(12) 0.0197(3) Uani 1 1 d . . . . .
C1 C 0.7879(2) 0.47002(16) 0.74835(15) 0.0208(4) Uani 1 1 d . . . . .
C2 C 0.6773(2) 0.52195(16) 0.67477(14) 0.0207(4) Uani 1 1 d . . . . .
C3 C 0.5315(2) 0.48415(16) 0.73658(14) 0.0199(4) Uani 1 1 d . . . . .
C4 C 0.5563(2) 0.42215(15) 0.83079(14) 0.0182(4) Uani 1 1 d . . . . .
C5 C 0.4437(2) 0.37921(15) 0.90598(14) 0.0198(4) Uani 1 1 d . . . . .
H5 H 0.462020 0.337863 0.968044 0.024 Uiso 1 1 calc R . . . .
C6 C 0.3004(2) 0.40124(16) 0.88383(15) 0.0219(4) Uani 1 1 d . . . . .
C7 C 0.2695(2) 0.46364(17) 0.79267(16) 0.0253(4) Uani 1 1 d . . . . .
H7 H 0.171854 0.477171 0.781209 0.030 Uiso 1 1 calc R . . . .
C8 C 0.3871(2) 0.50595(17) 0.71817(16) 0.0244(4) Uani 1 1 d . . . . .
H8 H 0.368464 0.548468 0.656662 0.029 Uiso 1 1 calc R . . . .
C9 C 0.6596(2) 0.65833(16) 0.66200(15) 0.0223(4) Uani 1 1 d . . . . .
C10 C 0.7247(2) 0.68471(18) 0.55888(16) 0.0276(4) Uani 1 1 d . . . . .
H10 H 0.730464 0.762334 0.531794 0.033 Uiso 1 1 calc R . . . .
C11 C 0.7843(3) 0.57566(18) 0.49634(16) 0.0289(4) Uani 1 1 d . . . . .
H11 H 0.835000 0.572687 0.423332 0.035 Uiso 1 1 calc R . . . .
C12 C 0.7561(2) 0.47852(17) 0.55894(15) 0.0230(4) Uani 1 1 d . . . . .
C13 C 0.8003(2) 0.35157(17) 0.52481(16) 0.0249(4) Uani 1 1 d . . . . .
C14 C 0.8993(3) 0.32139(19) 0.42236(17) 0.0314(5) Uani 1 1 d . . . . .
H14 H 0.938112 0.381497 0.378115 0.038 Uiso 1 1 calc R . . . .
C15 C 0.9396(3) 0.2038(2) 0.38639(18) 0.0382(5) Uani 1 1 d . . . . .
H15 H 1.005232 0.185462 0.318175 0.046 Uiso 1 1 calc R . . . .
C16 C 0.8836(3) 0.1131(2) 0.4507(2) 0.0403(5) Uani 1 1 d . . . . .
H16 H 0.909727 0.034247 0.425487 0.048 Uiso 1 1 calc R . . . .
C17 C 0.7885(3) 0.1401(2) 0.5528(2) 0.0469(6) Uani 1 1 d . . . . .
H17 H 0.751700 0.079149 0.596903 0.056 Uiso 1 1 calc R . . . .
C18 C 0.7479(3) 0.2583(2) 0.58942(19) 0.0393(5) Uani 1 1 d . . . . .
H18 H 0.684446 0.275464 0.658464 0.047 Uiso 1 1 calc R . . . .
C19 C 0.7739(2) 0.35434(16) 0.92200(15) 0.0210(4) Uani 1 1 d . . . . .
H19A H 0.697242 0.372483 0.990205 0.025 Uiso 1 1 calc R . . . .
H19B H 0.860686 0.387552 0.923460 0.025 Uiso 1 1 calc R . . . .
C20 C 0.8268(2) 0.21824(17) 0.90996(15) 0.0218(4) Uani 1 1 d . . . . .
C21 C 0.9526(3) 0.16857(19) 0.82657(17) 0.0314(5) Uani 1 1 d . . . . .
H21 H 1.003241 0.219334 0.777373 0.038 Uiso 1 1 calc R . . . .
C22 C 1.0027(3) 0.0439(2) 0.81647(19) 0.0373(5) Uani 1 1 d . . . . .
H22 H 1.087041 0.011303 0.760697 0.045 Uiso 1 1 calc R . . . .
C23 C 0.9279(3) -0.03226(19) 0.88883(19) 0.0356(5) Uani 1 1 d . . . . .
H23 H 0.961446 -0.115929 0.881526 0.043 Uiso 1 1 calc R . . . .
C24 C 0.8037(3) 0.01585(19) 0.97175(19) 0.0348(5) Uani 1 1 d . . . . .
H24 H 0.753568 -0.035384 1.020730 0.042 Uiso 1 1 calc R . . . .
C25 C 0.7530(2) 0.14087(18) 0.98246(17) 0.0286(4) Uani 1 1 d . . . . .
H25 H 0.669004 0.172885 1.038680 0.034 Uiso 1 1 calc R . . . .
C26 C 0.5935(2) 0.73888(17) 0.75455(15) 0.0234(4) Uani 1 1 d . . . . .
C27 C 0.5397(2) 0.87190(17) 0.73650(16) 0.0260(4) Uani 1 1 d . . . . .
C28 C 0.5600(3) 0.9515(2) 0.80611(18) 0.0363(5) Uani 1 1 d . . . . .
H28 H 0.611696 0.921550 0.858698 0.044 Uiso 1 1 calc R . . . .
C29 C 0.5030(3) 1.0752(2) 0.7966(2) 0.0489(7) Uani 1 1 d . . . . .
H29 H 0.518374 1.128268 0.842006 0.059 Uiso 1 1 calc R . . . .
C30 C 0.4239(3) 1.1199(2) 0.7205(2) 0.0517(7) Uani 1 1 d . . . . .
H30 H 0.384899 1.202898 0.715140 0.062 Uiso 1 1 calc R . . . .
C31 C 0.4023(3) 1.0413(2) 0.6518(2) 0.0456(6) Uani 1 1 d . . . . .
H31 H 0.348124 1.071785 0.600653 0.055 Uiso 1 1 calc R . . . .
C32 C 0.4611(3) 0.91749(19) 0.65892(17) 0.0326(5) Uani 1 1 d . . . . .
H32 H 0.447968 0.865128 0.611868 0.039 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C6 1.8986(19) . ?
O1 C1 1.212(2) . ?
O2 C26 1.221(2) . ?
N1 C1 1.365(2) . ?
N1 C4 1.400(2) . ?
N1 C19 1.465(2) . ?
C1 C2 1.563(2) . ?
C2 C3 1.511(3) . ?
C2 C9 1.518(2) . ?
C2 C12 1.535(3) . ?
C3 C4 1.400(2) . ?
C3 C8 1.382(3) . ?
C4 C5 1.374(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(3) . ?
C6 C7 1.385(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.397(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.345(3) . ?
C9 C26 1.463(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.441(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.348(3) . ?
C12 C13 1.469(3) . ?
C13 C14 1.403(3) . ?
C13 C18 1.392(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.378(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.380(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.381(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.387(3) . ?
C18 H18 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.512(2) . ?
C20 C21 1.391(3) . ?
C20 C25 1.387(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.385(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.380(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.376(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.390(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.494(3) . ?
C27 C28 1.397(3) . ?
C27 C32 1.389(3) . ?
C28 H28 0.9300 . ?
C28 C29 1.386(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.373(4) . ?
C30 H30 0.9300 . ?
C30 C31 1.386(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.387(3) . ?
C32 H32 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C4 112.01(15) . . ?
C1 N1 C19 123.38(15) . . ?
C4 N1 C19 124.55(15) . . ?
O1 C1 N1 126.02(17) . . ?
O1 C1 C2 126.45(17) . . ?
N1 C1 C2 107.52(15) . . ?
C3 C2 C1 101.83(14) . . ?
C3 C2 C9 113.82(15) . . ?
C3 C2 C12 119.98(16) . . ?
C9 C2 C1 109.78(15) . . ?
C9 C2 C12 102.12(15) . . ?
C12 C2 C1 109.24(15) . . ?
C4 C3 C2 108.83(16) . . ?
C8 C3 C2 131.74(17) . . ?
C8 C3 C4 119.33(17) . . ?
C3 C4 N1 109.77(16) . . ?
C5 C4 N1 127.31(16) . . ?
C5 C4 C3 122.93(17) . . ?
C4 C5 H5 122.0 . . ?
C4 C5 C6 116.09(17) . . ?
C6 C5 H5 122.0 . . ?
C5 C6 Br1 116.68(14) . . ?
C7 C6 Br1 120.14(15) . . ?
C7 C6 C5 123.18(18) . . ?
C6 C7 H7 120.5 . . ?
C6 C7 C8 118.97(18) . . ?
C8 C7 H7 120.5 . . ?
C3 C8 C7 119.49(17) . . ?
C3 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C10 C9 C2 108.89(16) . . ?
C10 C9 C26 129.23(18) . . ?
C26 C9 C2 121.63(16) . . ?
C9 C10 H10 124.8 . . ?
C9 C10 C11 110.38(17) . . ?
C11 C10 H10 124.8 . . ?
C10 C11 H11 124.9 . . ?
C12 C11 C10 110.20(17) . . ?
C12 C11 H11 124.9 . . ?
C11 C12 C2 108.30(16) . . ?
C11 C12 C13 126.43(18) . . ?
C13 C12 C2 125.19(17) . . ?
C14 C13 C12 119.26(18) . . ?
C18 C13 C12 123.07(18) . . ?
C18 C13 C14 117.66(19) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.9(2) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.6(2) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.2 . . ?
C15 C16 C17 119.6(2) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(2) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 H18 119.4 . . ?
C17 C18 C13 121.2(2) . . ?
C17 C18 H18 119.4 . . ?
N1 C19 H19A 109.1 . . ?
N1 C19 H19B 109.1 . . ?
N1 C19 C20 112.50(14) . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C21 C20 C19 120.26(18) . . ?
C25 C20 C19 120.85(17) . . ?
C25 C20 C21 118.88(18) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.3(2) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.3(2) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 120.1 . . ?
C24 C23 C22 119.9(2) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.1(2) . . ?
C25 C24 H24 119.9 . . ?
C20 C25 C24 120.50(19) . . ?
C20 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
O2 C26 C9 120.13(17) . . ?
O2 C26 C27 120.21(17) . . ?
C9 C26 C27 119.66(16) . . ?
C28 C27 C26 117.95(19) . . ?
C32 C27 C26 122.28(18) . . ?
C32 C27 C28 119.60(19) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.8(2) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(2) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 120.0 . . ?
C29 C30 C31 120.1(2) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.9 . . ?
C30 C31 C32 120.3(2) . . ?
C32 C31 H31 119.9 . . ?
C27 C32 H32 120.1 . . ?
C31 C32 C27 119.8(2) . . ?
C31 C32 H32 120.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.284
_oxdiff_exptl_absorpt_empirical_full_min 0.625
####################################################################### 
# 
# 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_exp_2605
_database_code_depnum_ccdc_archive 'CCDC 2180633'
loop_
_audit_author_name
_audit_author_address
'Sunewang Rixin Wang'
;East China Normal University
China
;
_audit_update_record             
;
2022-06-21 deposited with the CCDC.	2022-10-02 downloaded from the CCDC.
;
_audit_creation_date             2022-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H22 Br N O2'
_chemical_formula_sum            'C32 H22 Br N O2'
_chemical_formula_weight         532.41
_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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   9.70430(10)
_cell_length_b                   17.15680(10)
_cell_length_c                   14.49380(10)
_cell_angle_alpha                90
_cell_angle_beta                 98.3360(10)
_cell_angle_gamma                90
_cell_volume                     2387.65(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14954
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.2370
_cell_measurement_theta_min      3.9820
_shelx_estimated_absorpt_T_max   0.682
_shelx_estimated_absorpt_T_min   0.531
_exptl_absorpt_coefficient_mu    2.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24261
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         4.018
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  16.00   1.00    1.00    --    0.00  37.00   0.00   35
  2  ω      0.00  26.00   1.00    1.00    --    0.00  37.00-150.00   26
  3  ω     46.00  89.00   1.00    1.00    --    0.00  37.00-150.00   43
  4  ω    -89.00 -33.00   1.00    1.00    --    0.00 -37.00 120.00   56
  5  ω     -8.00  18.00   1.00    1.00    --    0.00 -37.00 120.00   26
  6  ω    -41.00  10.00   1.00    1.00    --    0.00 -57.00  30.00   51
  7  ω     46.00  89.00   1.00    1.00    --    0.00  37.00   0.00   43
  8  ω      6.00 111.00   1.00    1.00    --   95.80 -61.00  30.00  105
  9  ω     46.00 101.00   1.00    1.00    --   95.80 -61.00-180.00   55
 10  ω     85.00 110.00   1.00    1.00    --   95.80 -82.00  90.00   25
 11  ω     11.00 127.00   1.00    1.00    --   95.80 -82.00-180.00  116
 12  ω     72.00 107.00   1.00    1.00    --   95.80 -82.00 -90.00   35
 13  ω     74.00 128.00   1.00    1.00    --   95.80 -82.00-120.00   54
 14  ω     69.00 162.00   1.00    1.00    --   95.80  15.00 -60.00   93
 15  ω     25.00  98.00   1.00    1.00    --   95.80 -45.00  30.00   73
 16  ω      6.00  42.00   1.00    1.00    --   95.80 -61.00-180.00   36
 17  ω      6.00 111.00   1.00    1.00    --   95.80 -82.00  30.00  105
 18  ω     85.00 185.00   1.00    1.00    --   95.80  61.00 -30.00  100
 19  ω    105.00 185.00   1.00    1.00    --   95.80  61.00 120.00   80
 20  ω     17.00 102.00   1.00    1.00    --   95.80 -82.00 -30.00   85
 21  ω     11.00 111.00   1.00    1.00    --   95.80 -30.00-180.00  100
 22  ω     83.00 111.00   1.00    1.00    --   95.80 -61.00  60.00   28
 23  ω    141.00 166.00   1.00    1.00    --   95.80  77.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0852113000
_diffrn_orient_matrix_UB_12      0.0234796000
_diffrn_orient_matrix_UB_13      0.0939675000
_diffrn_orient_matrix_UB_21      0.1357815000
_diffrn_orient_matrix_UB_22      -0.0180445000
_diffrn_orient_matrix_UB_23      -0.0391130000
_diffrn_orient_matrix_UB_31      0.0052882000
_diffrn_orient_matrix_UB_32      0.0848068000
_diffrn_orient_matrix_UB_33      -0.0343862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3982
_reflns_number_total             4262
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0261
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0339P)²+1.1098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0702
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.18699(2) 0.73803(2) 0.66875(2) 0.03732(8) Uani 1 1 d . . . . .
O1 O 0.32137(14) 0.74945(7) 0.41761(8) 0.0332(3) Uani 1 1 d . . . . .
H1 H 0.355364 0.710786 0.396443 0.050 Uiso 1 1 calc GR . . . .
O2 O 0.43634(12) 0.63277(7) 0.36450(8) 0.0303(3) Uani 1 1 d . . . . .
N1 N 0.60477(14) 0.54495(8) 0.41867(9) 0.0231(3) Uani 1 1 d . . . . .
C1 C 0.25564(17) 0.83196(10) 0.62369(11) 0.0262(3) Uani 1 1 d . . . . .
C2 C 0.22512(19) 0.90089(11) 0.66609(13) 0.0343(4) Uani 1 1 d . . . . .
H2 H 0.176212 0.900174 0.716719 0.041 Uiso 1 1 calc R . . . .
C3 C 0.2681(2) 0.97064(11) 0.63241(14) 0.0386(4) Uani 1 1 d . . . . .
H3 H 0.247954 1.017231 0.660411 0.046 Uiso 1 1 calc R . . . .
C4 C 0.3407(2) 0.97155(11) 0.55743(15) 0.0409(5) Uani 1 1 d . . . . .
H4 H 0.368681 1.018720 0.534536 0.049 Uiso 1 1 calc R . . . .
C5 C 0.37188(19) 0.90229(10) 0.51628(13) 0.0340(4) Uani 1 1 d . . . . .
H5 H 0.421171 0.903391 0.465844 0.041 Uiso 1 1 calc R . . . .
C6 C 0.33088(16) 0.83109(9) 0.54895(11) 0.0246(3) Uani 1 1 d . . . . .
C7 C 0.37610(17) 0.75906(9) 0.50406(11) 0.0239(3) Uani 1 1 d . . . . .
C8 C 0.47786(16) 0.71211(9) 0.55223(11) 0.0224(3) Uani 1 1 d . . . . .
C9 C 0.55020(16) 0.64565(9) 0.52023(10) 0.0214(3) Uani 1 1 d . . . . .
C10 C 0.52610(16) 0.60882(9) 0.43149(11) 0.0238(3) Uani 1 1 d . . . . .
C11 C 0.71052(16) 0.51714(9) 0.48772(11) 0.0222(3) Uani 1 1 d . . . . .
C12 C 0.78793(18) 0.45155(10) 0.47044(12) 0.0279(4) Uani 1 1 d . . . . .
H12 H 0.769025 0.426360 0.413188 0.033 Uiso 1 1 calc R . . . .
C13 C 0.89192(19) 0.42360(10) 0.53700(12) 0.0297(4) Uani 1 1 d . . . . .
H13 H 0.942056 0.379567 0.524631 0.036 Uiso 1 1 calc R . . . .
C14 C 0.92222(18) 0.46108(10) 0.62279(12) 0.0294(4) Uani 1 1 d . . . . .
H14 H 0.993450 0.442675 0.667338 0.035 Uiso 1 1 calc R . . . .
C15 C 0.84641(17) 0.52533(10) 0.64126(11) 0.0256(3) Uani 1 1 d . . . . .
H15 H 0.866685 0.549557 0.699041 0.031 Uiso 1 1 calc R . . . .
C16 C 0.73901(16) 0.55562(9) 0.57544(11) 0.0214(3) Uani 1 1 d . . . . .
C17 C 0.65486(16) 0.62217(9) 0.59088(10) 0.0206(3) Uani 1 1 d . . . . .
C18 C 0.54283(16) 0.72534(9) 0.64597(11) 0.0220(3) Uani 1 1 d . . . . .
H18 H 0.516717 0.764119 0.684797 0.026 Uiso 1 1 calc R . . . .
C19 C 0.64879(16) 0.67316(9) 0.67091(10) 0.0203(3) Uani 1 1 d . . . . .
C20 C 0.73510(16) 0.67779(8) 0.76430(11) 0.0209(3) Uani 1 1 d . . . . .
C21 C 0.87931(17) 0.68645(9) 0.77558(12) 0.0263(3) Uani 1 1 d . . . . .
H21 H 0.925466 0.682597 0.723836 0.032 Uiso 1 1 calc R . . . .
C22 C 0.95537(19) 0.70073(10) 0.86267(13) 0.0330(4) Uani 1 1 d . . . . .
H22 H 1.051375 0.707341 0.868753 0.040 Uiso 1 1 calc R . . . .
C23 C 0.8879(2) 0.70510(11) 0.94050(12) 0.0359(4) Uani 1 1 d . . . . .
H23 H 0.938626 0.714213 0.999026 0.043 Uiso 1 1 calc R . . . .
C24 C 0.7450(2) 0.69585(11) 0.93084(12) 0.0343(4) Uani 1 1 d . . . . .
H24 H 0.699778 0.698381 0.983130 0.041 Uiso 1 1 calc R . . . .
C25 C 0.66850(18) 0.68283(10) 0.84365(11) 0.0263(3) Uani 1 1 d . . . . .
H25 H 0.572274 0.677402 0.837831 0.032 Uiso 1 1 calc R . . . .
C26 C 0.57729(17) 0.50500(10) 0.32725(11) 0.0262(3) Uani 1 1 d . . . . .
H26A H 0.485447 0.519678 0.296526 0.031 Uiso 1 1 calc R . . . .
H26B H 0.577132 0.449126 0.337464 0.031 Uiso 1 1 calc R . . . .
C27 C 0.68316(17) 0.52422(9) 0.26385(11) 0.0235(3) Uani 1 1 d . . . . .
C28 C 0.71748(18) 0.60104(10) 0.24708(12) 0.0286(4) Uani 1 1 d . . . . .
H28 H 0.679161 0.641244 0.278108 0.034 Uiso 1 1 calc R . . . .
C29 C 0.8083(2) 0.61818(11) 0.18450(12) 0.0334(4) Uani 1 1 d . . . . .
H29 H 0.829472 0.669841 0.173074 0.040 Uiso 1 1 calc R . . . .
C30 C 0.86765(19) 0.55905(11) 0.13899(12) 0.0344(4) Uani 1 1 d . . . . .
H30 H 0.928150 0.570802 0.096721 0.041 Uiso 1 1 calc R . . . .
C31 C 0.8368(2) 0.48262(11) 0.15645(12) 0.0363(4) Uani 1 1 d . . . . .
H31 H 0.878230 0.442594 0.126983 0.044 Uiso 1 1 calc R . . . .
C32 C 0.74404(19) 0.46517(10) 0.21799(12) 0.0309(4) Uani 1 1 d . . . . .
H32 H 0.722426 0.413433 0.228616 0.037 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C1 1.8958(17) . ?
O1 C7 1.299(2) . ?
O2 C10 1.2748(19) . ?
N1 C10 1.364(2) . ?
N1 C11 1.409(2) . ?
N1 C26 1.4812(19) . ?
C1 C2 1.384(2) . ?
C1 C6 1.391(2) . ?
C2 C3 1.380(3) . ?
C3 C4 1.378(3) . ?
C4 C5 1.383(3) . ?
C5 C6 1.389(2) . ?
C6 C7 1.492(2) . ?
C7 C8 1.383(2) . ?
C8 C9 1.450(2) . ?
C8 C18 1.431(2) . ?
C9 C10 1.422(2) . ?
C9 C17 1.393(2) . ?
C11 C12 1.396(2) . ?
C11 C16 1.424(2) . ?
C12 C13 1.377(2) . ?
C13 C14 1.393(2) . ?
C14 C15 1.373(2) . ?
C15 C16 1.406(2) . ?
C16 C17 1.440(2) . ?
C17 C19 1.461(2) . ?
C18 C19 1.372(2) . ?
C19 C20 1.487(2) . ?
C20 C21 1.393(2) . ?
C20 C25 1.401(2) . ?
C21 C22 1.388(2) . ?
C22 C23 1.386(3) . ?
C23 C24 1.383(3) . ?
C24 C25 1.388(2) . ?
C26 C27 1.511(2) . ?
C27 C28 1.389(2) . ?
C27 C32 1.390(2) . ?
C28 C29 1.385(3) . ?
C29 C30 1.381(3) . ?
C30 C31 1.377(3) . ?
C31 C32 1.389(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
C10 N1 C11 122.67(13) . . ?
C10 N1 C26 117.52(13) . . ?
C11 N1 C26 119.80(13) . . ?
C2 C1 Br1 117.69(13) . . ?
C2 C1 C6 121.67(16) . . ?
C6 C1 Br1 120.62(12) . . ?
C3 C2 C1 119.26(17) . . ?
C4 C3 C2 120.27(17) . . ?
C3 C4 C5 119.95(18) . . ?
C4 C5 C6 121.15(17) . . ?
C1 C6 C7 124.69(15) . . ?
C5 C6 C1 117.68(15) . . ?
C5 C6 C7 117.57(15) . . ?
O1 C7 C6 114.90(14) . . ?
O1 C7 C8 125.14(15) . . ?
C8 C7 C6 119.74(14) . . ?
C7 C8 C9 129.80(15) . . ?
C7 C8 C18 124.84(15) . . ?
C18 C8 C9 105.15(13) . . ?
C10 C9 C8 127.96(14) . . ?
C17 C9 C8 109.12(13) . . ?
C17 C9 C10 122.91(14) . . ?
O2 C10 N1 119.30(14) . . ?
O2 C10 C9 123.41(15) . . ?
N1 C10 C9 117.29(14) . . ?
N1 C11 C16 120.31(14) . . ?
C12 C11 N1 120.08(14) . . ?
C12 C11 C16 119.61(15) . . ?
C13 C12 C11 120.92(15) . . ?
C12 C13 C14 120.20(16) . . ?
C15 C14 C13 119.67(16) . . ?
C14 C15 C16 121.98(15) . . ?
C11 C16 C17 117.73(14) . . ?
C15 C16 C11 117.60(14) . . ?
C15 C16 C17 124.66(14) . . ?
C9 C17 C16 118.98(14) . . ?
C9 C17 C19 107.54(13) . . ?
C16 C17 C19 133.42(14) . . ?
C19 C18 C8 110.92(14) . . ?
C17 C19 C20 132.26(14) . . ?
C18 C19 C17 107.25(13) . . ?
C18 C19 C20 120.45(14) . . ?
C21 C20 C19 122.42(14) . . ?
C21 C20 C25 118.17(15) . . ?
C25 C20 C19 118.98(14) . . ?
C22 C21 C20 121.20(16) . . ?
C23 C22 C21 119.87(17) . . ?
C24 C23 C22 119.76(16) . . ?
C23 C24 C25 120.45(17) . . ?
C24 C25 C20 120.53(16) . . ?
N1 C26 C27 113.13(13) . . ?
C28 C27 C26 120.99(15) . . ?
C28 C27 C32 118.59(16) . . ?
C32 C27 C26 120.37(15) . . ?
C29 C28 C27 120.50(16) . . ?
C30 C29 C28 120.39(17) . . ?
C31 C30 C29 119.70(17) . . ?
C30 C31 C32 120.11(16) . . ?
C31 C32 C27 120.68(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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.803
####################################################################### 
# 
# 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_exp_2213
_database_code_depnum_ccdc_archive 'CCDC 2180635'
loop_
_audit_author_name
_audit_author_address
'Sunewang Rixin Wang'
;East China Normal University
China
;
_audit_update_record             
;
2022-06-21 deposited with the CCDC.	2022-10-02 downloaded from the CCDC.
;
_audit_creation_date             2021-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H24 O5'
_chemical_formula_sum            'C28 H24 O5'
_chemical_formula_weight         440.47
_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'
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                   11.6432(4)
_cell_length_b                   26.6464(11)
_cell_length_c                   7.3107(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.172(4)
_cell_angle_gamma                90
_cell_volume                     2217.15(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5302
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      74.0490
_cell_measurement_theta_min      3.8720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11384
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.317
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_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      8.00  34.00   1.00    1.00    --    0.00  38.00  60.00   26
  2  ω     48.00  89.00   1.00    1.00    --    0.00  77.00 -90.00   41
  3  ω    -28.00  31.00   1.00    1.00    --    0.00  77.00 -90.00   59
  4  ω     52.00  86.00   1.00    1.00    --    0.00  38.00  60.00   34
  5  ω     75.00 101.00   1.00    1.00    --   95.80 -77.00 150.00   26
  6  ω     92.00 118.00   1.00    1.00    --   95.80 -82.00 150.00   26
  7  ω    129.00 163.00   1.00    1.00    --   95.80  82.00-150.00   34
  8  ω     35.00 127.00   1.00    1.00    --   95.80 -82.00  30.00   92
  9  ω     77.00 181.00   1.00    1.00    --   95.80  30.00 -90.00  104
 10  ω     26.00  74.00   1.00    1.00    --   95.80 -77.00 150.00   48
 11  ω     76.00 157.00   1.00    1.00    --   95.80  45.00   0.00   81
 12  ω     76.00 121.00   1.00    1.00    --   95.80 -82.00  90.00   45
 13  ω     64.00 115.00   1.00    1.00    --   95.80  82.00-150.00   51
 14  ω     26.00 109.00   1.00    1.00    --   95.80 -45.00  90.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0226652000
_diffrn_orient_matrix_UB_12      -0.0520112000
_diffrn_orient_matrix_UB_13      0.0776577000
_diffrn_orient_matrix_UB_21      -0.0607441000
_diffrn_orient_matrix_UB_22      0.0250886000
_diffrn_orient_matrix_UB_23      0.1442420000
_diffrn_orient_matrix_UB_31      -0.1187454000
_diffrn_orient_matrix_UB_32      -0.0029113000
_diffrn_orient_matrix_UB_33      -0.1401763000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3342
_reflns_number_total             3946
_reflns_odcompleteness_completeness 99.70
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         3946
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0433
_refine_ls_restrained_S_all      1.074
_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)+(0.0641P)²+0.1615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1181
_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 Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C3(H3), C6(H6), C18(H18), C24(H24), C27(H27), C22(H22),
 C28(H28), C5(H5), C25(H25), C26(H26), C21(H21), C20(H20), C19(H19)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
O5 O 0.56225(8) 0.53487(4) 0.23646(14) 0.0305(3) Uani 1 1 d . . . . .
O2 O 0.50397(9) 0.32009(4) 0.08767(14) 0.0355(3) Uani 1 1 d . . . . .
O3 O 0.64864(9) 0.30903(4) 0.53460(16) 0.0400(3) Uani 1 1 d . . . . .
O1 O 0.12951(9) 0.28274(5) 0.21567(17) 0.0481(3) Uani 1 1 d . . . . .
O4 O 0.77587(9) 0.36777(4) 0.48404(17) 0.0453(3) Uani 1 1 d . . . . .
C13 C 0.46184(12) 0.45960(5) 0.27335(19) 0.0290(3) Uani 1 1 d . . . . .
H13 H 0.390787 0.442596 0.259847 0.035 Uiso 1 1 calc R . . . .
C1 C 0.45381(12) 0.35478(5) 0.35554(19) 0.0275(3) Uani 1 1 d . . . . .
C14 C 0.46027(12) 0.50789(5) 0.22165(19) 0.0274(3) Uani 1 1 d . . . . .
C15 C 0.66686(12) 0.51185(6) 0.31232(19) 0.0285(3) Uani 1 1 d . . . . .
C7 C 0.56766(12) 0.38264(6) 0.39196(19) 0.0285(3) Uani 1 1 d . . . . .
C17 C 0.35559(12) 0.53839(6) 0.14397(19) 0.0281(3) Uani 1 1 d . . . . .
C12 C 0.56972(12) 0.43272(6) 0.34950(18) 0.0279(3) Uani 1 1 d . . . . .
C2 C 0.42203(12) 0.32414(5) 0.19575(19) 0.0288(3) Uani 1 1 d . . . . .
C23 C 0.76698(12) 0.54580(5) 0.3142(2) 0.0287(3) Uani 1 1 d . . . . .
C16 C 0.67341(12) 0.46402(6) 0.36951(19) 0.0295(3) Uani 1 1 d . . . . .
H16 H 0.746360 0.450525 0.423444 0.035 Uiso 1 1 calc R . . . .
C8 C 0.67500(12) 0.35475(6) 0.4711(2) 0.0321(3) Uani 1 1 d . . . . .
C3 C 0.31382(13) 0.30038(6) 0.1550(2) 0.0321(3) Uani 1 1 d . . . . .
H3 H 0.293789 0.280112 0.049541 0.039 Uiso 1 1 calc R . . . .
C4 C 0.23531(12) 0.30689(6) 0.2721(2) 0.0339(4) Uani 1 1 d . . . . .
C6 C 0.37430(12) 0.35951(6) 0.4697(2) 0.0314(3) Uani 1 1 d . . . . .
H6 H 0.394625 0.379111 0.576938 0.038 Uiso 1 1 calc R . . . .
C18 C 0.24275(13) 0.51935(6) 0.1337(2) 0.0347(4) Uani 1 1 d . . . . .
H18 H 0.233246 0.487162 0.177485 0.042 Uiso 1 1 calc R . . . .
C24 C 0.76153(12) 0.58294(6) 0.1777(2) 0.0335(3) Uani 1 1 d . . . . .
H24 H 0.693102 0.587066 0.086860 0.040 Uiso 1 1 calc R . . . .
C27 C 0.96435(12) 0.57255(6) 0.4502(2) 0.0366(4) Uani 1 1 d . . . . .
H27 H 1.032328 0.569286 0.542652 0.044 Uiso 1 1 calc R . . . .
C22 C 0.36696(13) 0.58667(6) 0.0772(2) 0.0331(3) Uani 1 1 d . . . . .
H22 H 0.441403 0.600170 0.084026 0.040 Uiso 1 1 calc R . . . .
C28 C 0.86983(12) 0.54124(6) 0.4515(2) 0.0331(3) Uani 1 1 d . . . . .
H28 H 0.874792 0.516995 0.544291 0.040 Uiso 1 1 calc R . . . .
C5 C 0.26444(12) 0.33614(6) 0.4316(2) 0.0342(4) Uani 1 1 d . . . . .
H5 H 0.212381 0.340124 0.511086 0.041 Uiso 1 1 calc R . . . .
C25 C 0.85729(13) 0.61362(6) 0.1769(2) 0.0372(4) Uani 1 1 d . . . . .
H25 H 0.853316 0.637766 0.083885 0.045 Uiso 1 1 calc R . . . .
C26 C 0.95873(13) 0.60865(6) 0.3130(2) 0.0381(4) Uani 1 1 d . . . . .
H26 H 1.022771 0.629454 0.312234 0.046 Uiso 1 1 calc R . . . .
C21 C 0.26872(14) 0.61476(6) 0.0008(2) 0.0392(4) Uani 1 1 d . . . . .
H21 H 0.277543 0.646768 -0.044986 0.047 Uiso 1 1 calc R . . . .
C10 C 0.47321(15) 0.29009(7) -0.0779(2) 0.0415(4) Uani 1 1 d . . . . .
H10A H 0.401866 0.302623 -0.154994 0.062 Uiso 1 1 calc GR . . . .
H10B H 0.461926 0.255933 -0.043838 0.062 Uiso 1 1 calc GR . . . .
H10C H 0.535205 0.291605 -0.145970 0.062 Uiso 1 1 calc GR . . . .
C20 C 0.15768(14) 0.59556(7) -0.0078(2) 0.0411(4) Uani 1 1 d . . . . .
H20 H 0.091702 0.614614 -0.058414 0.049 Uiso 1 1 calc R . . . .
C19 C 0.14513(13) 0.54787(7) 0.0592(2) 0.0419(4) Uani 1 1 d . . . . .
H19 H 0.070384 0.534881 0.054131 0.050 Uiso 1 1 calc R . . . .
C9 C 0.74796(15) 0.27939(7) 0.6214(3) 0.0476(4) Uani 1 1 d . . . . .
H9A H 0.796033 0.272706 0.532484 0.071 Uiso 1 1 calc GR . . . .
H9B H 0.721266 0.248262 0.663888 0.071 Uiso 1 1 calc GR . . . .
H9C H 0.793097 0.297358 0.726147 0.071 Uiso 1 1 calc GR . . . .
C11 C 0.04287(14) 0.29077(8) 0.3231(3) 0.0513(5) Uani 1 1 d . . . . .
H11A H -0.027218 0.272676 0.268199 0.077 Uiso 1 1 calc GR . . . .
H11B H 0.025454 0.325953 0.325249 0.077 Uiso 1 1 calc GR . . . .
H11C H 0.071794 0.279114 0.448659 0.077 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O5 C14 1.3727(16) . ?
O5 C15 1.3721(16) . ?
O2 C2 1.3653(17) . ?
O2 C10 1.4317(18) . ?
O3 C8 1.3616(18) . ?
O3 C9 1.4334(18) . ?
O1 C4 1.3739(17) . ?
O1 C11 1.419(2) . ?
O4 C8 1.2090(17) . ?
C13 H13 0.9300 . ?
C13 C14 1.340(2) . ?
C13 C12 1.4511(19) . ?
C1 C7 1.4934(18) . ?
C1 C2 1.409(2) . ?
C1 C6 1.377(2) . ?
C14 C17 1.4754(19) . ?
C15 C23 1.4735(19) . ?
C15 C16 1.338(2) . ?
C7 C12 1.372(2) . ?
C7 C8 1.4642(19) . ?
C17 C18 1.3956(19) . ?
C17 C22 1.392(2) . ?
C12 C16 1.4490(19) . ?
C2 C3 1.385(2) . ?
C23 C24 1.397(2) . ?
C23 C28 1.396(2) . ?
C16 H16 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.389(2) . ?
C4 C5 1.384(2) . ?
C6 H6 0.9300 . ?
C6 C5 1.397(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.380(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.384(2) . ?
C27 H27 0.9300 . ?
C27 C28 1.383(2) . ?
C27 C26 1.382(2) . ?
C22 H22 0.9300 . ?
C22 C21 1.382(2) . ?
C28 H28 0.9300 . ?
C5 H5 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.381(2) . ?
C26 H26 0.9300 . ?
C21 H21 0.9300 . ?
C21 C20 1.379(2) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C20 H20 0.9300 . ?
C20 C19 1.381(2) . ?
C19 H19 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 O5 C14 118.49(11) . . ?
C2 O2 C10 116.92(11) . . ?
C8 O3 C9 115.16(12) . . ?
C4 O1 C11 117.37(13) . . ?
C14 C13 H13 118.6 . . ?
C14 C13 C12 122.76(13) . . ?
C12 C13 H13 118.6 . . ?
C2 C1 C7 120.26(12) . . ?
C6 C1 C7 122.10(12) . . ?
C6 C1 C2 117.58(13) . . ?
O5 C14 C17 111.87(12) . . ?
C13 C14 O5 121.37(12) . . ?
C13 C14 C17 126.76(13) . . ?
O5 C15 C23 111.24(12) . . ?
C16 C15 O5 122.64(12) . . ?
C16 C15 C23 126.08(13) . . ?
C12 C7 C1 120.04(12) . . ?
C12 C7 C8 121.94(13) . . ?
C8 C7 C1 118.02(12) . . ?
C18 C17 C14 120.82(13) . . ?
C22 C17 C14 120.80(13) . . ?
C22 C17 C18 118.37(14) . . ?
C7 C12 C13 120.80(13) . . ?
C7 C12 C16 126.23(13) . . ?
C16 C12 C13 112.96(12) . . ?
O2 C2 C1 115.61(12) . . ?
O2 C2 C3 123.67(13) . . ?
C3 C2 C1 120.72(13) . . ?
C24 C23 C15 120.77(13) . . ?
C28 C23 C15 120.68(13) . . ?
C28 C23 C24 118.55(13) . . ?
C15 C16 C12 121.67(13) . . ?
C15 C16 H16 119.2 . . ?
C12 C16 H16 119.2 . . ?
O3 C8 C7 110.71(12) . . ?
O4 C8 O3 121.01(14) . . ?
O4 C8 C7 128.28(14) . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.83(13) . . ?
C4 C3 H3 120.1 . . ?
O1 C4 C3 114.90(13) . . ?
O1 C4 C5 124.19(13) . . ?
C5 C4 C3 120.90(13) . . ?
C1 C6 H6 118.6 . . ?
C1 C6 C5 122.86(14) . . ?
C5 C6 H6 118.6 . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.56(14) . . ?
C19 C18 H18 119.7 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.42(14) . . ?
C25 C24 H24 119.8 . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C26 C27 C28 120.59(14) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 C17 120.67(14) . . ?
C21 C22 H22 119.7 . . ?
C23 C28 H28 119.8 . . ?
C27 C28 C23 120.41(14) . . ?
C27 C28 H28 119.8 . . ?
C4 C5 C6 118.08(14) . . ?
C4 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.52(15) . . ?
C26 C25 H25 119.7 . . ?
C27 C26 H26 120.3 . . ?
C25 C26 C27 119.50(14) . . ?
C25 C26 H26 120.3 . . ?
C22 C21 H21 119.8 . . ?
C20 C21 C22 120.37(15) . . ?
C20 C21 H21 119.8 . . ?
O2 C10 H10A 109.5 . . ?
O2 C10 H10B 109.5 . . ?
O2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C21 C20 H20 120.2 . . ?
C21 C20 C19 119.56(15) . . ?
C19 C20 H20 120.2 . . ?
C18 C19 C20 120.46(15) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C11 H11A 109.5 . . ?
O1 C11 H11B 109.5 . . ?
O1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.238
_oxdiff_exptl_absorpt_empirical_full_min 0.398
####################################################################### 
# 
# 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_exp_2341
_database_code_depnum_ccdc_archive 'CCDC 2180634'
loop_
_audit_author_name
_audit_author_address
'Sunewang Rixin Wang'
;East China Normal University
China
;
_audit_update_record             
;
2022-06-21 deposited with the CCDC.	2022-10-02 downloaded from the CCDC.
;
_audit_creation_date             2021-11-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H36 O6'
_chemical_formula_sum            'C42 H36 O6'
_chemical_formula_weight         636.71
_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'
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                   14.4529(2)
_cell_length_b                   14.2698(3)
_cell_length_c                   17.1004(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.845(2)
_cell_angle_gamma                90
_cell_volume                     3337.74(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7230
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.2920
_cell_measurement_theta_min      4.1060
_shelx_estimated_absorpt_T_max   0.866
_shelx_estimated_absorpt_T_min   0.793
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18112
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.231
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00 -21.00   1.00    1.00    --    0.00 -37.00-120.00   26
  2  ω    -83.00 -39.00   1.00    1.00    --    0.00 -37.00 -60.00   44
  3  ω    -78.00  19.00   1.00    1.00    --    0.00 -37.00  90.00   97
  4  ω    -33.00  17.00   1.00    1.00    --    0.00 -37.00 -60.00   50
  5  ω     72.00 166.00   1.00    3.00    --   95.80  15.00  90.00   94
  6  ω     27.00 128.00   1.00    3.00    --   95.80 -82.00   0.00  101
  7  ω     16.00 104.00   1.00    3.00    --   95.80 -82.00 -60.00   88
  8  ω     81.00 117.00   1.00    3.00    --   95.80  30.00 120.00   36
  9  ω      7.00 120.00   1.00    3.00    --   95.80 -61.00   0.00  113
 10  ω     66.00 109.00   1.00    3.00    --   95.80 -82.00-120.00   43
 11  ω     76.00 184.00   1.00    3.00    --   95.80  30.00 -30.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0191157000
_diffrn_orient_matrix_UB_12      0.1033693000
_diffrn_orient_matrix_UB_13      0.0158033000
_diffrn_orient_matrix_UB_21      0.0396444000
_diffrn_orient_matrix_UB_22      0.0302264000
_diffrn_orient_matrix_UB_23      -0.0696165000
_diffrn_orient_matrix_UB_31      -0.1037077000
_diffrn_orient_matrix_UB_32      -0.0075423000
_diffrn_orient_matrix_UB_33      -0.0629378000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4801
_reflns_number_total             5872
_reflns_odcompleteness_completeness 99.73
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5872
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.1494
_refine_ls_restrained_S_all      0.903
_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)+(0.0415P)²+30.4148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2764
_refine_ls_wR_factor_ref         0.2840
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 C41, C42, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C28, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C29, C28, O5, C27, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C36, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C39 \\sim C38 \\sim C37 \\sim C42 \\sim C41 \\sim C40: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C28 \\sim C29: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O6 \\sim C27 \\sim C28 \\sim O5 \\sim C29: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C41) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C40) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C39) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C38) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C37) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C22(H22)
4.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C28(H28A,H28B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C19(H19), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C39(H39), C40(H40), C41(H41), C42(H42), C37(H37)
4.d Fitted hexagon refined as free rotating group:
 C38(C39,C40,C41,C42,C37)
4.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C29(H29A,H29B,H29C)
4.f Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 -0.0271(4) 0.2177(4) 0.1405(3) 0.0659(13) Uani 1 1 d . . . . .
H1 H -0.046773 0.248148 0.097597 0.099 Uiso 1 1 calc GR . . . .
O2 O -0.0830(3) 0.3091(3) 0.0090(3) 0.0651(13) Uani 1 1 d . . . . .
O3 O -0.0640(3) 0.2972(3) -0.1142(2) 0.0510(10) Uani 1 1 d . . . . .
O4 O 0.3473(6) 0.3100(4) -0.1194(4) 0.117(3) Uani 1 1 d . . . . .
O5 O 0.4644(4) 0.1404(6) 0.1150(4) 0.133(2) Uani 1 1 d . U . . .
O6 O 0.4336(3) 0.0037(5) 0.0619(4) 0.1011(17) Uani 1 1 d . U . . .
C1 C 0.0602(4) 0.0870(4) 0.2032(3) 0.0439(13) Uani 1 1 d . . . . .
C2 C 0.0927(5) 0.1241(6) 0.2833(4) 0.0618(17) Uani 1 1 d . . . . .
H2 H 0.102878 0.188186 0.291327 0.074 Uiso 1 1 calc R . . . .
C3 C 0.1094(5) 0.0649(8) 0.3500(4) 0.078(2) Uani 1 1 d . . . . .
H3 H 0.132684 0.089083 0.403347 0.094 Uiso 1 1 calc R . . . .
C4 C 0.0917(5) -0.0304(7) 0.3383(5) 0.079(3) Uani 1 1 d . . . . .
H4 H 0.100953 -0.069669 0.383594 0.095 Uiso 1 1 calc R . . . .
C5 C 0.0604(4) -0.0671(5) 0.2592(5) 0.0644(19) Uani 1 1 d . . . . .
H5 H 0.049603 -0.131180 0.251192 0.077 Uiso 1 1 calc R . . . .
C6 C 0.0451(4) -0.0078(5) 0.1916(4) 0.0508(15) Uani 1 1 d . . . . .
H6 H 0.024632 -0.032406 0.138336 0.061 Uiso 1 1 calc R . . . .
C7 C 0.2128(3) 0.0262(4) 0.1221(3) 0.0352(11) Uani 1 1 d . . . . .
C8 C 0.2704(4) 0.0586(4) 0.1995(3) 0.0433(13) Uani 1 1 d . . . . .
H8 H 0.270173 0.121891 0.212316 0.052 Uiso 1 1 calc R . . . .
C9 C 0.3279(4) -0.0033(5) 0.2572(4) 0.0547(15) Uani 1 1 d . . . . .
H9 H 0.364805 0.018500 0.309208 0.066 Uiso 1 1 calc R . . . .
C10 C 0.3311(5) -0.0969(5) 0.2384(4) 0.0606(17) Uani 1 1 d . . . . .
H10 H 0.370017 -0.138033 0.277541 0.073 Uiso 1 1 calc R . . . .
C11 C 0.2764(5) -0.1294(4) 0.1614(4) 0.0562(16) Uani 1 1 d . . . . .
H11 H 0.279383 -0.192330 0.148240 0.067 Uiso 1 1 calc R . . . .
C12 C 0.2167(4) -0.0685(4) 0.1036(4) 0.0444(13) Uani 1 1 d . . . . .
H12 H 0.179164 -0.091036 0.052100 0.053 Uiso 1 1 calc R . . . .
C13 C 0.1500(3) 0.0913(4) 0.0596(3) 0.0348(11) Uani 1 1 d . . . . .
C14 C 0.0697(4) 0.1490(4) 0.0661(3) 0.0371(11) Uani 1 1 d . . . . .
C15 C 0.0368(4) 0.2034(4) -0.0097(3) 0.0362(11) Uani 1 1 d . . . . .
C16 C 0.0939(3) 0.1795(4) -0.0567(3) 0.0373(11) Uani 1 1 d . . . . .
H16 H 0.087692 0.203950 -0.108570 0.045 Uiso 1 1 calc R . . . .
C17 C 0.1642(3) 0.1115(4) -0.0140(3) 0.0353(11) Uani 1 1 d . . . . .
C18 C 0.2445(4) 0.0749(4) -0.0446(3) 0.0383(12) Uani 1 1 d . . . . .
H18 H 0.258470 0.009557 -0.027118 0.046 Uiso 1 1 calc R . . . .
C19 C 0.2224(4) 0.0812(4) -0.1363(3) 0.0400(12) Uani 1 1 d . . . . .
H19 H 0.164524 0.058786 -0.173766 0.048 Uiso 1 1 calc R . . . .
C20 C 0.2918(4) 0.1211(4) -0.1597(3) 0.0382(12) Uani 1 1 d . . . . .
C21 C 0.3777(4) 0.1494(5) -0.0861(3) 0.0469(14) Uani 1 1 d . . . . .
H21 H 0.434049 0.108980 -0.081387 0.056 Uiso 1 1 calc R . . . .
C22 C 0.3401(4) 0.1342(4) -0.0100(3) 0.0417(13) Uani 1 1 d . . . . .
H22 H 0.325044 0.194825 0.009955 0.050 Uiso 1 1 calc R . . . .
C23 C 0.0349(4) 0.1523(4) 0.1327(4) 0.0460(14) Uani 1 1 d . . . . .
C24 C -0.0404(4) 0.2721(4) -0.0352(4) 0.0444(13) Uani 1 1 d . . . . .
C25 C -0.1375(5) 0.3708(5) -0.1440(4) 0.0632(18) Uani 1 1 d . . . . .
H25A H -0.108551 0.431979 -0.127330 0.076 Uiso 1 1 calc R . . . .
H25B H -0.190504 0.362201 -0.121444 0.076 Uiso 1 1 calc R . . . .
C26 C -0.1744(5) 0.3634(6) -0.2352(4) 0.071(2) Uani 1 1 d . . . . .
H26A H -0.224480 0.409470 -0.257156 0.106 Uiso 1 1 calc GR . . . .
H26B H -0.200926 0.301956 -0.250748 0.106 Uiso 1 1 calc GR . . . .
H26C H -0.121644 0.374050 -0.256735 0.106 Uiso 1 1 calc GR . . . .
C27 C 0.4155(4) 0.0840(7) 0.0578(4) 0.0705(16) Uani 1 1 d . U . . .
C28 C 0.5390(8) 0.0873(11) 0.1838(6) 0.155(4) Uani 1 1 d . U . . .
H28A H 0.513760 0.026257 0.191503 0.186 Uiso 1 1 calc R . . . .
H28B H 0.598939 0.078670 0.170763 0.186 Uiso 1 1 calc R . . . .
C29 C 0.5567(6) 0.1422(7) 0.2561(5) 0.093(3) Uani 1 1 d . U . . .
H29A H 0.577752 0.203653 0.246466 0.140 Uiso 1 1 calc GR . . . .
H29B H 0.606708 0.113076 0.300792 0.140 Uiso 1 1 calc GR . . . .
H29C H 0.497711 0.147021 0.270134 0.140 Uiso 1 1 calc GR . . . .
C30 C 0.2926(4) 0.1293(4) -0.2453(3) 0.0435(13) Uani 1 1 d . . . . .
C31 C 0.2061(5) 0.1273(5) -0.3123(4) 0.0562(16) Uani 1 1 d . . . . .
H31 H 0.146316 0.125335 -0.302736 0.067 Uiso 1 1 calc R . . . .
C32 C 0.2082(5) 0.1281(5) -0.3924(4) 0.0649(19) Uani 1 1 d . . . . .
H32 H 0.149604 0.125664 -0.435929 0.078 Uiso 1 1 calc R . . . .
C33 C 0.2927(6) 0.1324(6) -0.4092(4) 0.078(2) Uani 1 1 d . . . . .
H33 H 0.293158 0.131195 -0.463427 0.094 Uiso 1 1 calc R . . . .
C34 C 0.3785(6) 0.1384(9) -0.3443(5) 0.110(4) Uani 1 1 d . . . . .
H34 H 0.437653 0.143117 -0.354755 0.132 Uiso 1 1 calc R . . . .
C35 C 0.3779(5) 0.1377(7) -0.2640(4) 0.088(3) Uani 1 1 d . . . . .
H35 H 0.436852 0.142933 -0.221150 0.106 Uiso 1 1 calc R . . . .
C36 C 0.4058(8) 0.2527(6) -0.0874(5) 0.091(2) Uani 1 1 d . U . . .
C38 C 0.5153(5) 0.2734(7) -0.0394(5) 0.129(2) Uani 1 1 d . U . . .
C39 C 0.5828(7) 0.2026(5) -0.0064(5) 0.137(2) Uani 1 1 d G U . . .
H39 H 0.563937 0.140146 -0.015325 0.164 Uiso 1 1 calc R . . . .
C40 C 0.6783(6) 0.2252(6) 0.0399(5) 0.140(2) Uani 1 1 d G U . . .
H40 H 0.723435 0.177902 0.061940 0.168 Uiso 1 1 calc R . . . .
C41 C 0.7064(5) 0.3186(7) 0.0532(5) 0.144(2) Uani 1 1 d G U . . .
H41 H 0.770369 0.333728 0.084146 0.172 Uiso 1 1 calc R . . . .
C42 C 0.6390(7) 0.3893(5) 0.0202(5) 0.140(2) Uani 1 1 d G U . . .
H42 H 0.657806 0.451799 0.029087 0.168 Uiso 1 1 calc R . . . .
C37 C 0.5434(6) 0.3667(6) -0.0261(5) 0.137(2) Uani 1 1 d G U . . .
H37 H 0.498307 0.414045 -0.048178 0.165 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.8200 . ?
O1 C23 1.330(7) . ?
O2 C24 1.236(7) . ?
O3 C24 1.331(7) . ?
O3 C25 1.463(7) . ?
O4 C36 1.177(12) . ?
O5 C27 1.287(11) . ?
O5 C28 1.516(11) . ?
O6 C27 1.172(10) . ?
C1 C2 1.399(8) . ?
C1 C6 1.375(9) . ?
C1 C23 1.473(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.377(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.387(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.384(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.396(7) . ?
C7 C12 1.393(7) . ?
C7 C13 1.483(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(8) . ?
C9 H9 0.9300 . ?
C9 C10 1.378(10) . ?
C10 H10 0.9300 . ?
C10 C11 1.379(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.388(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.456(7) . ?
C13 C17 1.371(7) . ?
C14 C15 1.453(7) . ?
C14 C23 1.386(7) . ?
C15 C16 1.368(7) . ?
C15 C24 1.443(7) . ?
C16 H16 0.9300 . ?
C16 C17 1.425(7) . ?
C17 C18 1.511(7) . ?
C18 H18 0.9800 . ?
C18 C19 1.499(7) . ?
C18 C22 1.565(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.324(7) . ?
C20 C21 1.509(7) . ?
C20 C30 1.472(7) . ?
C21 H21 0.9800 . ?
C21 C22 1.578(7) . ?
C21 C36 1.531(10) . ?
C22 H22 0.9800 . ?
C22 C27 1.494(8) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.480(10) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.415(13) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.396(8) . ?
C30 C35 1.375(9) . ?
C31 H31 0.9300 . ?
C31 C32 1.381(9) . ?
C32 H32 0.9300 . ?
C32 C33 1.343(10) . ?
C33 H33 0.9300 . ?
C33 C34 1.374(10) . ?
C34 H34 0.9300 . ?
C34 C35 1.376(10) . ?
C35 H35 0.9300 . ?
C36 C38 1.558(11) . ?
C38 C39 1.3900 . ?
C38 C37 1.3900 . ?
C39 H39 0.9300 . ?
C39 C40 1.3900 . ?
C40 H40 0.9300 . ?
C40 C41 1.3900 . ?
C41 H41 0.9300 . ?
C41 C42 1.3900 . ?
C42 H42 0.9300 . ?
C42 C37 1.3900 . ?
C37 H37 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C23 O1 H1 109.5 . . ?
C24 O3 C25 117.8(5) . . ?
C27 O5 C28 110.8(9) . . ?
C2 C1 C23 118.6(6) . . ?
C6 C1 C2 120.1(6) . . ?
C6 C1 C23 121.2(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.6(7) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(7) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(7) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.8(7) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 120.2(6) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C8 C7 C13 121.0(5) . . ?
C12 C7 C8 118.7(5) . . ?
C12 C7 C13 120.3(5) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.2(6) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.6(6) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.8(6) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(6) . . ?
C12 C11 H11 119.9 . . ?
C7 C12 H12 119.7 . . ?
C11 C12 C7 120.5(6) . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C7 128.0(4) . . ?
C17 C13 C7 123.7(4) . . ?
C17 C13 C14 108.1(4) . . ?
C15 C14 C13 105.9(4) . . ?
C23 C14 C13 126.3(5) . . ?
C23 C14 C15 127.9(5) . . ?
C16 C15 C14 107.8(4) . . ?
C16 C15 C24 123.1(5) . . ?
C24 C15 C14 129.1(5) . . ?
C15 C16 H16 125.2 . . ?
C15 C16 C17 109.5(5) . . ?
C17 C16 H16 125.2 . . ?
C13 C17 C16 108.7(4) . . ?
C13 C17 C18 127.2(5) . . ?
C16 C17 C18 124.0(5) . . ?
C17 C18 H18 109.2 . . ?
C17 C18 C22 111.5(4) . . ?
C19 C18 C17 114.4(4) . . ?
C19 C18 H18 109.2 . . ?
C19 C18 C22 103.1(4) . . ?
C22 C18 H18 109.2 . . ?
C18 C19 H19 122.7 . . ?
C20 C19 C18 114.6(5) . . ?
C20 C19 H19 122.7 . . ?
C19 C20 C21 111.3(5) . . ?
C19 C20 C30 125.8(5) . . ?
C30 C20 C21 122.7(5) . . ?
C20 C21 H21 110.5 . . ?
C20 C21 C22 104.0(4) . . ?
C20 C21 C36 113.3(6) . . ?
C22 C21 H21 110.5 . . ?
C36 C21 H21 110.5 . . ?
C36 C21 C22 107.9(5) . . ?
C18 C22 C21 105.1(4) . . ?
C18 C22 H22 109.9 . . ?
C21 C22 H22 109.9 . . ?
C27 C22 C18 111.6(5) . . ?
C27 C22 C21 110.3(4) . . ?
C27 C22 H22 109.9 . . ?
O1 C23 C1 111.1(5) . . ?
O1 C23 C14 122.7(5) . . ?
C14 C23 C1 126.2(5) . . ?
O2 C24 O3 119.4(5) . . ?
O2 C24 C15 126.5(5) . . ?
O3 C24 C15 114.1(5) . . ?
O3 C25 H25A 110.4 . . ?
O3 C25 H25B 110.4 . . ?
O3 C25 C26 106.8(6) . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
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 . . ?
O5 C27 C22 111.9(8) . . ?
O6 C27 O5 120.6(7) . . ?
O6 C27 C22 127.4(8) . . ?
O5 C28 H28A 110.4 . . ?
O5 C28 H28B 110.4 . . ?
H28A C28 H28B 108.6 . . ?
C29 C28 O5 106.5(9) . . ?
C29 C28 H28A 110.4 . . ?
C29 C28 H28B 110.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C20 121.4(5) . . ?
C35 C30 C20 122.2(5) . . ?
C35 C30 C31 116.3(6) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.9(6) . . ?
C32 C31 H31 119.6 . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.7(6) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 120.8 . . ?
C32 C33 C34 118.5(7) . . ?
C34 C33 H33 120.8 . . ?
C33 C34 H34 119.7 . . ?
C33 C34 C35 120.7(7) . . ?
C35 C34 H34 119.7 . . ?
C30 C35 C34 121.9(7) . . ?
C30 C35 H35 119.1 . . ?
C34 C35 H35 119.1 . . ?
O4 C36 C21 121.5(8) . . ?
O4 C36 C38 124.6(8) . . ?
C21 C36 C38 113.9(9) . . ?
C39 C38 C36 122.4(7) . . ?
C39 C38 C37 120.0 . . ?
C37 C38 C36 117.5(7) . . ?
C38 C39 H39 120.0 . . ?
C38 C39 C40 120.0 . . ?
C40 C39 H39 120.0 . . ?
C39 C40 H40 120.0 . . ?
C39 C40 C41 120.0 . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C41 C42 H42 120.0 . . ?
C37 C42 C41 120.0 . . ?
C37 C42 H42 120.0 . . ?
C38 C37 H37 120.0 . . ?
C42 C37 C38 120.0 . . ?
C42 C37 H37 120.0 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 17.7 0.1 ?
2 0.000 0.500 0.000 17.7 0.1 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.226
_oxdiff_exptl_absorpt_empirical_full_min 0.727
