# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

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

data_rmji7
_database_code_depnum_ccdc_archive 'CCDC 1848231'
_audit_update_record             
;
2018-06-08 deposited with the CCDC.
2018-07-31 downloaded from the CCDC.
;
_audit_creation_date             2018-06-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H30.89 B Br0.11'
_chemical_formula_sum            'C39 H30.89 B Br0.11'
_chemical_formula_weight         518.93
_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'
B B 0.0090 0.0039 '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'

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

_cell_length_a                   10.71416(15)
_cell_length_b                   18.5823(3)
_cell_length_c                   14.07156(18)
_cell_angle_alpha                90
_cell_angle_beta                 95.4564(12)
_cell_angle_gamma                90
_cell_volume                     2788.87(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    24943
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.6090
_cell_measurement_theta_min      2.3590
_shelx_estimated_absorpt_T_max   0.913
_shelx_estimated_absorpt_T_min   0.795
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.7b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1095
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.133
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36142
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.410
_diffrn_reflns_theta_min         3.952
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     46.00  94.00   1.00    1.00    --    5.00  57.00  90.00   48
  2  ω     -9.00  18.00   1.00    1.00    --    5.00  57.00  90.00   27
  3  ω    -55.00  -6.00   1.00    1.00    --  -45.10 -76.00-120.00   49
  4  ω   -129.00 -82.00   1.00    1.00    --  -45.10 -50.00  56.56   47
  5  ω    -34.00  32.00   1.00    1.00    --  -45.10  64.00  -8.07   66
  6  ω    -53.00  43.00   1.00    1.00    --  -45.10  57.00 -30.00   96
  7  ω   -124.00 -82.00   1.00    1.00    --  -45.10 -76.00-120.00   42
  8  ω    -74.00   9.00   1.00    1.00    --  -45.10  61.00 173.36   83
  9  ω    -80.00 -54.00   1.00    1.00    --  -45.10  64.00  -8.07   26
 10  ω    -78.00  44.00   1.00    1.00    --  -45.10  57.00  90.00  122
 11  ω   -198.00 -79.00   1.00    1.00    -- -110.00 -57.00-150.00  119
 12  ω   -146.00-120.00   1.00    1.00    -- -110.00  38.00-150.00   26
 13  ω   -139.00-113.00   1.00    1.00    -- -110.00  76.00  30.00   26
 14  ω    -92.00 -62.00   1.00    1.00    -- -110.00  76.00  30.00   30
 15  ω   -138.00 -61.00   1.00    1.00    -- -110.00  76.00 120.00   77
 16  ω   -121.00 -22.00   1.00    1.00    -- -110.00  76.00 -60.00   99
 17  ω   -198.00 -75.00   1.00    1.00    -- -110.00 -64.00 -62.85  123
 18  ω   -138.00-112.00   1.00    1.00    -- -110.00  38.00  90.00   26
 19  ω   -143.00 -73.00   1.00    1.00    -- -110.00  76.00   0.00   70
 20  ω   -199.00 -72.00   1.00    1.00    -- -110.00 -76.00-120.00  127
 21  ω   -111.00 -70.00   1.00    1.00    -- -110.00 -75.00 -52.09   41
 22  ω   -106.00 -81.00   1.00    1.00    -- -110.00  38.00  90.00   25
 23  ω    -84.00 -22.00   1.00    1.00    -- -110.00  76.00-150.00   62
 24  ω    -91.00 -66.00   1.00    1.00    -- -110.00  38.00  60.00   25
 25  ω   -149.00 -61.00   1.00    1.00    -- -110.00  76.00  60.00   88
 26  ω   -119.00 -94.00   1.00    1.00    -- -110.00  57.00 -90.00   25
 27  ω    -98.00 -73.00   1.00    1.00    -- -110.00 -76.00 -60.00   25
 28  ω   -100.00 -70.00   1.00    1.00    -- -110.00 -76.00 -30.00   30
 29  ω   -157.00-131.00   1.00    1.00    -- -110.00 -57.00-180.00   26
 30  ω   -121.00 -78.00   1.00    1.00    -- -110.00 -57.00-180.00   43
 31  ω   -121.00 -95.00   1.00    1.00    -- -110.00  19.00-180.00   26
 32  ω   -192.00-133.00   1.00    1.00    -- -110.00  19.00-180.00   59
 33  ω   -199.00 -70.00   1.00    1.00    -- -110.00 -76.00 -34.89  129
 34  ω   -171.00 -75.00   1.00    1.00    -- -110.00 -76.00 150.00   96
 35  ω    -95.00 -70.00   1.00    1.00    -- -110.00 -75.00 -19.81   25
 36  ω   -177.00-144.00   1.00    1.00    -- -110.00 -75.00 -19.81   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525375000
_diffrn_orient_matrix_UB_12      0.0568365000
_diffrn_orient_matrix_UB_13      0.0652914000
_diffrn_orient_matrix_UB_21      -0.0977576000
_diffrn_orient_matrix_UB_22      -0.0547660000
_diffrn_orient_matrix_UB_23      0.0285870000
_diffrn_orient_matrix_UB_31      0.0924963000
_diffrn_orient_matrix_UB_32      -0.0254412000
_diffrn_orient_matrix_UB_33      0.0836924000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5487
_reflns_number_total             5791
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_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         0.233
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         5791
_refine_ls_number_restraints     1241
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0599
_refine_ls_restrained_S_all      1.077
_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)+(0.0410P)²+1.7964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1464
_refine_special_details          
'With only the mesityl group there are two large peaks near C3_3 and C5_3. These have been attributed to a small brominated impurity (see paper SI). In order to complete the model, two additional mesityl components were added, their relative atomic positions refined to be the same as the major mesityl component, their occupancies refined against that for the bromine present and their distance to the repective bromines fixed. Further flat and sadi restraints were introduced in order to refine sensible geometries around the mesityl C-B bond. The thermal parameters for all disordered components were restrained in order to refine sensible thermal ellipsoids.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Br3-C3_1 = Br1-C3_2
 1.9 with sigma of 0.01
 C2_1-Br3 \\sim Br3-C4_1
 with sigma of 0.02
 C6_1-B1 \\sim B1-C2_1
 with sigma of 0.02
 C1_1-B1 \\sim C1_3-B1 \\sim C1_2-B1
 with sigma of 0.001
3. Restrained planarity
 C1_2, C2_2, C3_2, C4_2, C5_2, C7_2, Br1, C8_2, C6_2, C9_2
 with sigma of 0.1
 Br3, C2_1, C3_1, C4_1, C5_1, C6_1, C8_1, C9_1, C1_1, C7_1
 with sigma of 0.1
 C6_1, C1_1, C2_1, B1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C34 \\sim C39 \\sim C35 \\sim C36 \\sim C38 \\sim C37 \\sim C35A \\sim C37A
\\sim C36A \\sim C38A \\sim C39A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C7_2 \\sim C2_3: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Br1 \\sim C5_1 \\sim C8_1 \\sim C8_2 \\sim C3_3 \\sim C8_3 \\sim C4_1 \\sim
C6_1 \\sim C9_1 \\sim C2_2 \\sim C3_2 \\sim C4_2 \\sim C7_2 \\sim C2_3 \\sim
C4_3 \\sim C7_3 \\sim Br3 \\sim C1_1 \\sim C2_1 \\sim C3_1 \\sim C7_1 \\sim
C1_2 \\sim C5_2 \\sim C6_2 \\sim C9_2 \\sim C1_3 \\sim C5_3 \\sim C6_3 \\sim
C9_3: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C39, C39A, C38, C38A, C37, C37A, C36, C36A, C35A, C35, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Br1, C5_1, C8_1, C8_2, C3_3, C8_3, C4_1, C6_1, C9_1, C2_2, C3_2, C4_2, C7_2,
 C2_3, C4_3, C7_3, Br3, C1_1, C2_1, C3_1, C7_1, C1_2, C5_2, C6_2, C9_2, C1_3,
 C5_3, C6_3, C9_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3, C9_3}
{C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1}
as
{C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2} sigma for 1-2: 0.01 1-3:
0.02
7. Others
 1*[Sof(Br3)+Sof(C1)+Sof(C2)+Sof(C3)+Sof(C4)+Sof(C5)+Sof(H5)+Sof(C6)+Sof(C7)+
 Sof(H7A)+Sof(H7B)+Sof(H7C)+Sof(C8)+Sof(H8A)+Sof(H8B)+Sof(H8C)+Sof(C9)+Sof(H9A)+
 Sof(H9B)+Sof(H9C)]+1*[Sof(Br1)+Sof(C1)+Sof(C2)+Sof(C3)+Sof(C4)+Sof(C5)+Sof(H5)+
 Sof(C6)+Sof(C7)+Sof(H7A)+Sof(H7B)+Sof(H7C)+Sof(C8)+Sof(H8A)+Sof(H8B)+Sof(H8C)+
 Sof(C9)+Sof(H9A)+Sof(H9B)+Sof(H9C)]+1*[Sof(C1)+Sof(C2)+Sof(C3)+Sof(H3)+Sof(C4)+
 Sof(C5)+Sof(H5)+Sof(C6)+Sof(C7)+Sof(H7A)+Sof(H7B)+Sof(H7C)+Sof(C8)+Sof(H8A)+
 Sof(H8B)+Sof(H8C)+Sof(C9)+Sof(H9A)+Sof(H9B)+Sof(H9C)]=1 with esd of 0.00001
 Sof(Br3)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(H9C)=FVAR(1)
 Sof(Br1)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(H9C)=FVAR(2)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(H9C)=FVAR(3)
 Sof(C39)=Sof(H39)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C38)=Sof(H38)=
 Sof(C37)=Sof(H37)=1-FVAR(4)
 Sof(C35A)=Sof(H35A)=Sof(C37A)=Sof(H37A)=Sof(C36A)=Sof(H36A)=Sof(C38A)=
 Sof(H38A)=Sof(C39A)=Sof(H39A)=FVAR(4)
8.a Riding coordinates:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
8.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B)
8.c Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
8.d Aromatic/amide H refined with riding coordinates:
 C28(H28), C11(H11), C17(H17), C13(H13), C22(H22), C12(H12), C15(H15),
 C16(H16), C25(H25), C23(H23), C24(H24), C39(H39), C35(H35), C36(H36), C38(H38),
  C37(H37), C35A(H35A), C37A(H37A), C36A(H36A), C38A(H38A), C39A(H39A), C5(H5),
 C3(H3), C5(H5), C5(H5)
8.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_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
C19 C 0.33358(16) 0.65619(9) 0.84531(12) 0.0293(4) Uani 1 1 d . . . . .
C29 C 0.52233(16) 0.63866(10) 0.70938(12) 0.0306(4) Uani 1 1 d . . . . .
C10 C 0.28939(16) 0.66040(10) 0.74643(12) 0.0298(4) Uani 1 1 d . . . . .
C20 C 0.55037(16) 0.61988(10) 0.80547(12) 0.0304(4) Uani 1 1 d . . . . .
C28 C 0.61643(16) 0.63255(10) 0.64546(12) 0.0329(4) Uani 1 1 d . . . . .
H28 H 0.597424 0.646663 0.582336 0.040 Uiso 1 1 calc R . . . .
C21 C 0.66415(16) 0.58008(10) 0.83206(13) 0.0326(4) Uani 1 1 d . . . . .
C26 C 0.75817(16) 0.57627(10) 0.76685(13) 0.0343(4) Uani 1 1 d . . . . .
C18 C 0.46256(16) 0.64075(10) 0.87581(12) 0.0312(4) Uani 1 1 d . . . . .
C27 C 0.73443(16) 0.60667(11) 0.67286(13) 0.0334(4) Uani 1 1 d . . . . .
C14 C 0.24877(17) 0.67105(10) 0.91511(12) 0.0335(4) Uani 1 1 d . . . . .
C11 C 0.16268(17) 0.67354(11) 0.72161(13) 0.0346(4) Uani 1 1 d . . . . .
H11 H 0.133555 0.676808 0.657355 0.042 Uiso 1 1 calc R . . . .
C17 C 0.50339(18) 0.65220(11) 0.97120(13) 0.0373(4) Uani 1 1 d . . . . .
H17 H 0.588239 0.647134 0.991029 0.045 Uiso 1 1 calc R . . . .
C30 C 0.82844(17) 0.60584(11) 0.60663(13) 0.0365(4) Uani 1 1 d . . . . .
C34 C 0.82611(18) 0.61708(11) 0.32855(14) 0.0383(4) Uani 1 1 d . U . . .
C13 C 0.12046(18) 0.68178(11) 0.88531(14) 0.0386(4) Uani 1 1 d . . . . .
H13 H 0.064199 0.688801 0.930869 0.046 Uiso 1 1 calc R . . . .
C22 C 0.68525(18) 0.53939(11) 0.91776(13) 0.0383(4) Uani 1 1 d . . . . .
H22 H 0.623030 0.537705 0.959511 0.046 Uiso 1 1 calc R . . . .
C12 C 0.07753(17) 0.68201(11) 0.79053(14) 0.0386(4) Uani 1 1 d . . . . .
H12 H -0.007530 0.687754 0.771974 0.046 Uiso 1 1 calc R . . . .
C31 C 0.90128(17) 0.60558(13) 0.54735(14) 0.0414(5) Uani 1 1 d . . . . .
C15 C 0.29564(19) 0.67831(12) 1.01226(13) 0.0416(5) Uani 1 1 d . . . . .
H15 H 0.240898 0.687978 1.058125 0.050 Uiso 1 1 calc R . . . .
C16 C 0.4208(2) 0.67116(12) 1.03864(13) 0.0438(5) Uani 1 1 d . . . . .
H16 H 0.451658 0.678916 1.101838 0.053 Uiso 1 1 calc R . . . .
C25 C 0.87176(18) 0.53936(12) 0.79368(15) 0.0429(5) Uani 1 1 d . . . . .
H25 H 0.934696 0.539193 0.752494 0.051 Uiso 1 1 calc R . . . .
C23 C 0.7950(2) 0.50261(12) 0.94032(15) 0.0455(5) Uani 1 1 d . . . . .
H23 H 0.806185 0.476483 0.996859 0.055 Uiso 1 1 calc R . . . .
C24 C 0.8905(2) 0.50410(13) 0.87872(16) 0.0492(5) Uani 1 1 d . . . . .
H24 H 0.966336 0.481082 0.895889 0.059 Uiso 1 1 calc R . . . .
B1 B 0.38545(18) 0.65732(11) 0.67164(13) 0.0296(4) Uani 1 1 d D . . . .
C39 C 0.7051(18) 0.6421(15) 0.3496(19) 0.039(3) Uani 0.46(2) 1 d . U P A 1
H39 H 0.701134 0.675984 0.397789 0.046 Uiso 0.46(2) 1 calc R . P A 1
C32 C 0.98798(19) 0.60735(17) 0.47293(15) 0.0560(7) Uani 1 1 d . . . . .
H32A H 1.004408 0.558440 0.453513 0.067 Uiso 1 1 calc R . . . .
H32B H 1.066878 0.628093 0.499263 0.067 Uiso 1 1 calc R . . . .
C33 C 0.9381(2) 0.65067(16) 0.38512(17) 0.0567(6) Uani 1 1 d . . . . .
H33A H 0.915015 0.698326 0.405500 0.068 Uiso 1 1 calc R . . . .
H33B H 1.004795 0.656257 0.343688 0.068 Uiso 1 1 calc R . . . .
C35 C 0.8195(15) 0.5601(10) 0.2564(12) 0.048(3) Uani 0.46(2) 1 d . U P A 1
H35 H 0.893660 0.538720 0.241419 0.058 Uiso 0.46(2) 1 calc R . P A 1
C36 C 0.7079(19) 0.5368(5) 0.2099(7) 0.054(3) Uani 0.46(2) 1 d . U P A 1
H36 H 0.707717 0.501096 0.163602 0.065 Uiso 0.46(2) 1 calc R . P A 1
C38 C 0.5983(11) 0.6191(8) 0.3034(12) 0.052(2) Uani 0.46(2) 1 d . U P A 1
H38 H 0.522999 0.638618 0.319232 0.063 Uiso 0.46(2) 1 calc R . P A 1
C37 C 0.5955(15) 0.5668(8) 0.2321(10) 0.057(3) Uani 0.46(2) 1 d . U P A 1
H37 H 0.519785 0.552316 0.200041 0.068 Uiso 0.46(2) 1 calc R . P A 1
C35A C 0.8575(11) 0.5668(8) 0.2669(11) 0.0445(19) Uani 0.54(2) 1 d . U P A 2
H35A H 0.941433 0.556118 0.262139 0.053 Uiso 0.54(2) 1 calc R . P A 2
C37A C 0.6414(14) 0.5485(7) 0.2146(7) 0.057(3) Uani 0.54(2) 1 d . U P A 2
H37A H 0.579525 0.524779 0.175646 0.068 Uiso 0.54(2) 1 calc R . P A 2
C36A C 0.7657(15) 0.5311(6) 0.2107(7) 0.055(2) Uani 0.54(2) 1 d . U P A 2
H36A H 0.787642 0.494972 0.169744 0.066 Uiso 0.54(2) 1 calc R . P A 2
C38A C 0.6092(11) 0.6017(8) 0.2769(9) 0.054(2) Uani 0.54(2) 1 d . U P A 2
H38A H 0.525960 0.614499 0.280879 0.065 Uiso 0.54(2) 1 calc R . P A 2
C39A C 0.708(2) 0.6359(14) 0.3347(17) 0.047(3) Uani 0.54(2) 1 d . U P A 2
H39A H 0.689620 0.671866 0.377112 0.056 Uiso 0.54(2) 1 calc R . P A 2
Br1 Br 0.2619(3) 0.56699(14) 0.31449(18) 0.0419(9) Uani 0.0806(10) 1 d D U P B
2
Br3 Br 0.2650(7) 0.7947(5) 0.3613(6) 0.049(3) Uani 0.0279(10) 1 d D U P B 1
C1_2 C 0.347(4) 0.6782(11) 0.5639(6) 0.030(4) Uani 0.0806(10) 1 d D U P B 2
C2_2 C 0.324(3) 0.6228(11) 0.4977(12) 0.031(3) Uani 0.0806(10) 1 d D U P B 2
C3_2 C 0.296(2) 0.6433(7) 0.4026(10) 0.031(3) Uani 0.0806(10) 1 d D U P B 2
C4_2 C 0.293(3) 0.7132(9) 0.3717(10) 0.029(3) Uani 0.0806(10) 1 d D U P B 2
C5_2 C 0.319(3) 0.7660(9) 0.4405(11) 0.033(4) Uani 0.0806(10) 1 d D U P B 2
H5_2 H 0.319845 0.813847 0.421077 0.039 Uiso 0.0806(10) 1 calc R . P B 2
C6_2 C 0.342(4) 0.7504(11) 0.5376(11) 0.031(3) Uani 0.0806(10) 1 d D U P B 2
C7_2 C 0.330(4) 0.5458(12) 0.528(2) 0.031(4) Uani 0.0806(10) 1 d D U P B 2
H7A_2 H 0.260781 0.519420 0.496937 0.046 Uiso 0.0806(10) 1 d R . P B 2
H7B_2 H 0.326501 0.543520 0.596127 0.046 Uiso 0.0806(10) 1 d R . P B 2
H7C_2 H 0.407291 0.525080 0.512157 0.046 Uiso 0.0806(10) 1 d R . P B 2
C8_2 C 0.260(2) 0.7350(13) 0.2690(10) 0.033(4) Uani 0.0806(10) 1 d D U P B 2
H8A_2 H 0.263328 0.786465 0.263788 0.050 Uiso 0.0806(10) 1 calc R . P B 2
H8B_2 H 0.318447 0.713752 0.229753 0.050 Uiso 0.0806(10) 1 calc R . P B 2
H8C_2 H 0.176681 0.718686 0.248177 0.050 Uiso 0.0806(10) 1 calc R . P B 2
C9_2 C 0.366(5) 0.8084(16) 0.6123(18) 0.052(7) Uani 0.0806(10) 1 d D U P B 2
H9A_2 H 0.359118 0.854801 0.582254 0.077 Uiso 0.0806(10) 1 calc R . P B 2
H9B_2 H 0.304759 0.804606 0.657818 0.077 Uiso 0.0806(10) 1 calc R . P B 2
H9C_2 H 0.448326 0.802712 0.644463 0.077 Uiso 0.0806(10) 1 calc R . P B 2
C1_3 C 0.3476(3) 0.66736(13) 0.56103(13) 0.0282(5) Uani 0.8915(14) 1 d D U P B
3
C2_3 C 0.3284(3) 0.60642(13) 0.50235(16) 0.0301(5) Uani 0.8915(14) 1 d D U P B
3
C3_3 C 0.2955(2) 0.61563(14) 0.40437(15) 0.0325(5) Uani 0.8915(14) 1 d D U P B
3
H3_3 H 0.283046 0.575136 0.365803 0.039 Uiso 0.8915(14) 1 calc R . P B 3
C4_3 C 0.2809(2) 0.68302(15) 0.36318(14) 0.0331(5) Uani 0.8915(14) 1 d D U P B
3
C5_3 C 0.3014(2) 0.74274(14) 0.42174(17) 0.0338(5) Uani 0.8915(14) 1 d D U P B
3
H5_3 H 0.292818 0.788451 0.395013 0.041 Uiso 0.8915(14) 1 calc R . P B 3
C6_3 C 0.3345(3) 0.73605(13) 0.51968(16) 0.0315(5) Uani 0.8915(14) 1 d D U P B
3
C7_3 C 0.3418(4) 0.53222(15) 0.5443(2) 0.0401(7) Uani 0.8915(14) 1 d D U P B 3
H7A_3 H 0.423430 0.527143 0.578096 0.060 Uiso 0.8915(14) 1 calc GR . P B 3
H7B_3 H 0.331508 0.497179 0.494035 0.060 Uiso 0.8915(14) 1 calc GR . P B 3
H7C_3 H 0.278878 0.524897 0.587593 0.060 Uiso 0.8915(14) 1 calc GR . P B 3
C8_3 C 0.2454(2) 0.69180(18) 0.25759(15) 0.0447(6) Uani 0.8915(14) 1 d D U P B
3
H8A_3 H 0.248224 0.645829 0.226751 0.067 Uiso 0.8915(14) 1 calc GR . P B 3
H8B_3 H 0.303178 0.724072 0.231470 0.067 Uiso 0.8915(14) 1 calc GR . P B 3
H8C_3 H 0.162062 0.711101 0.247286 0.067 Uiso 0.8915(14) 1 calc GR . P B 3
C9_3 C 0.3570(4) 0.80237(17) 0.5813(2) 0.0443(7) Uani 0.8915(14) 1 d D U P B 3
H9A_3 H 0.292260 0.806314 0.623692 0.067 Uiso 0.8915(14) 1 calc GR . P B 3
H9B_3 H 0.355934 0.844285 0.541307 0.067 Uiso 0.8915(14) 1 calc GR . P B 3
H9C_3 H 0.437032 0.798596 0.617839 0.067 Uiso 0.8915(14) 1 calc GR . P B 3
C1_1 C 0.364(3) 0.6475(9) 0.5597(2) 0.031(4) Uani 0.0279(10) 1 d D U P B 1
C2_1 C 0.347(3) 0.7125(10) 0.5120(10) 0.032(4) Uani 0.0279(10) 1 d D U P B 1
C3_1 C 0.2972(16) 0.7056(8) 0.4178(10) 0.033(3) Uani 0.0279(10) 1 d D U P B 1
C4_1 C 0.276(4) 0.6430(10) 0.3694(16) 0.034(4) Uani 0.0279(10) 1 d D U P B 1
C5_1 C 0.305(4) 0.5797(10) 0.4202(14) 0.033(4) Uani 0.0279(10) 1 d D U P B 1
H5_1 H 0.293124 0.535653 0.389135 0.040 Uiso 0.0279(10) 1 calc R . P B 1
C6_1 C 0.351(5) 0.5808(10) 0.5169(13) 0.030(4) Uani 0.0279(10) 1 d D U P B 1
C7_1 C 0.369(6) 0.7834(13) 0.560(2) 0.038(8) Uani 0.0279(10) 1 d D U P B 1
H7A_1 H 0.352223 0.821468 0.514865 0.057 Uiso 0.0279(10) 1 calc R . P B 1
H7B_1 H 0.314315 0.788119 0.610338 0.057 Uiso 0.0279(10) 1 calc R . P B 1
H7C_1 H 0.454622 0.786361 0.587382 0.057 Uiso 0.0279(10) 1 calc R . P B 1
C8_1 C 0.218(5) 0.638(2) 0.2676(18) 0.044(8) Uani 0.0279(10) 1 d D U P B 1
H8A_1 H 0.164651 0.596764 0.259421 0.066 Uiso 0.0279(10) 1 d R . P B 1
H8B_1 H 0.168061 0.681064 0.255911 0.066 Uiso 0.0279(10) 1 d R . P B 1
H8C_1 H 0.280442 0.636304 0.223281 0.066 Uiso 0.0279(10) 1 d R . P B 1
C9_1 C 0.383(5) 0.5125(13) 0.572(2) 0.037(9) Uani 0.0279(10) 1 d D U P B 1
H9A_1 H 0.368278 0.471748 0.530687 0.056 Uiso 0.0279(10) 1 calc R . P B 1
H9B_1 H 0.468998 0.513445 0.597575 0.056 Uiso 0.0279(10) 1 calc R . P B 1
H9C_1 H 0.330260 0.508776 0.623800 0.056 Uiso 0.0279(10) 1 calc R . P B 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C19 C10 1.429(2) . ?
C19 C18 1.436(2) . ?
C19 C14 1.427(2) . ?
C29 C20 1.401(2) . ?
C29 C28 1.418(2) . ?
C29 B1 1.551(3) . ?
C10 C11 1.391(2) . ?
C10 B1 1.541(2) . ?
C20 C21 1.444(2) . ?
C20 C18 1.481(2) . ?
C28 H28 0.9300 . ?
C28 C27 1.373(2) . ?
C21 C26 1.428(3) . ?
C21 C22 1.423(3) . ?
C26 C27 1.438(3) . ?
C26 C25 1.417(3) . ?
C18 C17 1.388(2) . ?
C27 C30 1.436(2) . ?
C14 C13 1.413(3) . ?
C14 C15 1.417(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.402(3) . ?
C17 H17 0.9300 . ?
C17 C16 1.403(3) . ?
C30 C31 1.195(3) . ?
C34 C39 1.434(19) . ?
C34 C33 1.510(3) . ?
C34 C35 1.464(17) . ?
C34 C35A 1.339(13) . ?
C34 C39A 1.32(2) . ?
C13 H13 0.9300 . ?
C13 C12 1.369(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.371(3) . ?
C12 H12 0.9300 . ?
C31 C32 1.465(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.364(3) . ?
C16 H16 0.9300 . ?
C25 H25 0.9300 . ?
C25 C24 1.362(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.403(3) . ?
C24 H24 0.9300 . ?
B1 C1_2 1.581(3) . ?
B1 C1_3 1.582(2) . ?
B1 C1_1 1.581(3) . ?
C39 H39 0.9300 . ?
C39 C38 1.33(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.528(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C35 H35 0.9300 . ?
C35 C36 1.377(13) . ?
C36 H36 0.9300 . ?
C36 C37 1.389(12) . ?
C38 H38 0.9300 . ?
C38 C37 1.395(12) . ?
C37 H37 0.9300 . ?
C35A H35A 0.9300 . ?
C35A C36A 1.373(9) . ?
C37A H37A 0.9300 . ?
C37A C36A 1.376(10) . ?
C37A C38A 1.387(11) . ?
C36A H36A 0.9300 . ?
C38A H38A 0.9300 . ?
C38A C39A 1.42(2) . ?
C39A H39A 0.9300 . ?
Br1 C3_2 1.897(9) . ?
Br3 C3_1 1.855(10) . ?
C1_2 C2_2 1.395(9) . ?
C1_2 C6_2 1.392(9) . ?
C2_2 C3_2 1.396(9) . ?
C2_2 C7_2 1.493(10) . ?
C3_2 C4_2 1.368(10) . ?
C4_2 C5_2 1.388(10) . ?
C4_2 C8_2 1.511(9) . ?
C5_2 H5_2 0.9300 . ?
C5_2 C6_2 1.397(9) . ?
C6_2 C9_2 1.510(10) . ?
C7_2 H7A_2 0.9599 . ?
C7_2 H7B_2 0.9600 . ?
C7_2 H7C_2 0.9599 . ?
C8_2 H8A_2 0.9600 . ?
C8_2 H8B_2 0.9600 . ?
C8_2 H8C_2 0.9600 . ?
C9_2 H9A_2 0.9600 . ?
C9_2 H9B_2 0.9600 . ?
C9_2 H9C_2 0.9600 . ?
C1_3 C2_3 1.405(3) . ?
C1_3 C6_3 1.404(3) . ?
C2_3 C3_3 1.401(3) . ?
C2_3 C7_3 1.501(3) . ?
C3_3 H3_3 0.9300 . ?
C3_3 C4_3 1.382(3) . ?
C4_3 C5_3 1.387(3) . ?
C4_3 C8_3 1.507(3) . ?
C5_3 H5_3 0.9300 . ?
C5_3 C6_3 1.396(3) . ?
C6_3 C9_3 1.513(3) . ?
C7_3 H7A_3 0.9600 . ?
C7_3 H7B_3 0.9600 . ?
C7_3 H7C_3 0.9600 . ?
C8_3 H8A_3 0.9600 . ?
C8_3 H8B_3 0.9600 . ?
C8_3 H8C_3 0.9600 . ?
C9_3 H9A_3 0.9600 . ?
C9_3 H9B_3 0.9600 . ?
C9_3 H9C_3 0.9600 . ?
C1_1 C2_1 1.386(9) . ?
C1_1 C6_1 1.378(9) . ?
C2_1 C3_1 1.387(9) . ?
C2_1 C7_1 1.492(10) . ?
C3_1 C4_1 1.356(10) . ?
C4_1 C5_1 1.397(10) . ?
C4_1 C8_1 1.510(10) . ?
C5_1 H5_1 0.9300 . ?
C5_1 C6_1 1.405(10) . ?
C6_1 C9_1 1.510(10) . ?
C7_1 H7A_1 0.9600 . ?
C7_1 H7B_1 0.9600 . ?
C7_1 H7C_1 0.9600 . ?
C8_1 H8A_1 0.9600 . ?
C8_1 H8B_1 0.9601 . ?
C8_1 H8C_1 0.9600 . ?
C9_1 H9A_1 0.9600 . ?
C9_1 H9B_1 0.9600 . ?
C9_1 H9C_1 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
C10 C19 C18 121.48(15) . . ?
C14 C19 C10 119.08(16) . . ?
C14 C19 C18 119.37(15) . . ?
C20 C29 C28 119.47(16) . . ?
C20 C29 B1 119.68(15) . . ?
C28 C29 B1 120.46(15) . . ?
C19 C10 B1 118.81(15) . . ?
C11 C10 C19 118.64(16) . . ?
C11 C10 B1 122.29(15) . . ?
C29 C20 C21 118.41(16) . . ?
C29 C20 C18 119.23(16) . . ?
C21 C20 C18 122.35(15) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 C29 122.76(16) . . ?
C27 C28 H28 118.6 . . ?
C26 C21 C20 119.25(16) . . ?
C22 C21 C20 123.62(16) . . ?
C22 C21 C26 116.96(17) . . ?
C21 C26 C27 119.84(16) . . ?
C25 C26 C21 119.58(17) . . ?
C25 C26 C27 120.50(17) . . ?
C19 C18 C20 120.46(15) . . ?
C17 C18 C19 117.65(16) . . ?
C17 C18 C20 121.65(16) . . ?
C28 C27 C26 118.25(16) . . ?
C28 C27 C30 120.36(17) . . ?
C30 C27 C26 121.26(16) . . ?
C13 C14 C19 119.23(16) . . ?
C13 C14 C15 121.23(17) . . ?
C15 C14 C19 119.46(17) . . ?
C10 C11 H11 119.0 . . ?
C10 C11 C12 121.99(17) . . ?
C12 C11 H11 119.0 . . ?
C18 C17 H17 118.9 . . ?
C18 C17 C16 122.12(18) . . ?
C16 C17 H17 118.9 . . ?
C31 C30 C27 176.2(2) . . ?
C39 C34 C33 116.5(9) . . ?
C39 C34 C35 113.1(11) . . ?
C35 C34 C33 130.4(7) . . ?
C35A C34 C33 113.2(5) . . ?
C39A C34 C33 124.9(9) . . ?
C39A C34 C35A 121.8(10) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 C14 121.13(17) . . ?
C12 C13 H13 119.4 . . ?
C21 C22 H22 119.2 . . ?
C23 C22 C21 121.65(18) . . ?
C23 C22 H22 119.2 . . ?
C11 C12 H12 120.2 . . ?
C13 C12 C11 119.55(17) . . ?
C13 C12 H12 120.2 . . ?
C30 C31 C32 177.9(2) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.17(17) . . ?
C16 C15 H15 119.9 . . ?
C17 C16 H16 119.7 . . ?
C15 C16 C17 120.50(17) . . ?
C15 C16 H16 119.7 . . ?
C26 C25 H25 119.4 . . ?
C24 C25 C26 121.19(19) . . ?
C24 C25 H25 119.4 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.46(19) . . ?
C24 C23 H23 119.8 . . ?
C25 C24 C23 119.83(19) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C29 B1 C1_2 122.3(14) . . ?
C29 B1 C1_3 120.58(19) . . ?
C29 B1 C1_1 111.1(11) . . ?
C10 B1 C29 116.46(15) . . ?
C10 B1 C1_2 121.0(14) . . ?
C10 B1 C1_3 122.84(19) . . ?
C10 B1 C1_1 129.8(12) . . ?
C34 C39 H39 118.4 . . ?
C38 C39 C34 123.2(16) . . ?
C38 C39 H39 118.4 . . ?
C31 C32 H32A 108.9 . . ?
C31 C32 H32B 108.9 . . ?
C31 C32 C33 113.15(19) . . ?
H32A C32 H32B 107.8 . . ?
C33 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C34 C33 C32 114.1(2) . . ?
C34 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
C32 C33 H33A 108.7 . . ?
C32 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C34 C35 H35 118.7 . . ?
C36 C35 C34 122.6(10) . . ?
C36 C35 H35 118.7 . . ?
C35 C36 H36 120.0 . . ?
C35 C36 C37 119.9(10) . . ?
C37 C36 H36 120.0 . . ?
C39 C38 H38 118.9 . . ?
C39 C38 C37 122.1(13) . . ?
C37 C38 H38 118.9 . . ?
C36 C37 C38 118.8(10) . . ?
C36 C37 H37 120.6 . . ?
C38 C37 H37 120.6 . . ?
C34 C35A H35A 120.0 . . ?
C34 C35A C36A 120.0(9) . . ?
C36A C35A H35A 120.0 . . ?
C36A C37A H37A 120.3 . . ?
C36A C37A C38A 119.5(8) . . ?
C38A C37A H37A 120.3 . . ?
C35A C36A C37A 120.4(9) . . ?
C35A C36A H36A 119.8 . . ?
C37A C36A H36A 119.8 . . ?
C37A C38A H38A 121.2 . . ?
C37A C38A C39A 117.6(11) . . ?
C39A C38A H38A 121.2 . . ?
C34 C39A C38A 120.6(14) . . ?
C34 C39A H39A 119.7 . . ?
C38A C39A H39A 119.7 . . ?
C2_2 C1_2 B1 118.2(12) . . ?
C6_2 C1_2 B1 119.4(13) . . ?
C6_2 C1_2 C2_2 122.4(9) . . ?
C1_2 C2_2 C3_2 116.5(9) . . ?
C1_2 C2_2 C7_2 121.0(12) . . ?
C3_2 C2_2 C7_2 122.6(12) . . ?
C2_2 C3_2 Br1 115.6(11) . . ?
C4_2 C3_2 Br1 120.3(10) . . ?
C4_2 C3_2 C2_2 124.1(10) . . ?
C3_2 C4_2 C5_2 116.9(9) . . ?
C3_2 C4_2 C8_2 123.7(12) . . ?
C5_2 C4_2 C8_2 119.3(12) . . ?
C4_2 C5_2 H5_2 118.6 . . ?
C4_2 C5_2 C6_2 122.7(11) . . ?
C6_2 C5_2 H5_2 118.6 . . ?
C1_2 C6_2 C5_2 117.3(10) . . ?
C1_2 C6_2 C9_2 120.3(12) . . ?
C5_2 C6_2 C9_2 122.4(12) . . ?
C2_2 C7_2 H7A_2 110.2 . . ?
C2_2 C7_2 H7B_2 108.9 . . ?
C2_2 C7_2 H7C_2 109.3 . . ?
H7A_2 C7_2 H7B_2 109.5 . . ?
H7A_2 C7_2 H7C_2 109.5 . . ?
H7B_2 C7_2 H7C_2 109.5 . . ?
C4_2 C8_2 H8A_2 109.5 . . ?
C4_2 C8_2 H8B_2 109.5 . . ?
C4_2 C8_2 H8C_2 109.5 . . ?
H8A_2 C8_2 H8B_2 109.5 . . ?
H8A_2 C8_2 H8C_2 109.5 . . ?
H8B_2 C8_2 H8C_2 109.5 . . ?
C6_2 C9_2 H9A_2 109.5 . . ?
C6_2 C9_2 H9B_2 109.5 . . ?
C6_2 C9_2 H9C_2 109.5 . . ?
H9A_2 C9_2 H9B_2 109.5 . . ?
H9A_2 C9_2 H9C_2 109.5 . . ?
H9B_2 C9_2 H9C_2 109.5 . . ?
C2_3 C1_3 B1 119.52(19) . . ?
C6_3 C1_3 B1 121.4(2) . . ?
C6_3 C1_3 C2_3 119.07(18) . . ?
C1_3 C2_3 C7_3 120.40(19) . . ?
C3_3 C2_3 C1_3 119.3(2) . . ?
C3_3 C2_3 C7_3 120.3(2) . . ?
C2_3 C3_3 H3_3 119.0 . . ?
C4_3 C3_3 C2_3 122.1(2) . . ?
C4_3 C3_3 H3_3 119.0 . . ?
C3_3 C4_3 C5_3 118.06(18) . . ?
C3_3 C4_3 C8_3 121.3(2) . . ?
C5_3 C4_3 C8_3 120.7(2) . . ?
C4_3 C5_3 H5_3 119.1 . . ?
C4_3 C5_3 C6_3 121.8(2) . . ?
C6_3 C5_3 H5_3 119.1 . . ?
C1_3 C6_3 C9_3 119.9(2) . . ?
C5_3 C6_3 C1_3 119.7(2) . . ?
C5_3 C6_3 C9_3 120.3(2) . . ?
C2_3 C7_3 H7A_3 109.5 . . ?
C2_3 C7_3 H7B_3 109.5 . . ?
C2_3 C7_3 H7C_3 109.5 . . ?
H7A_3 C7_3 H7B_3 109.5 . . ?
H7A_3 C7_3 H7C_3 109.5 . . ?
H7B_3 C7_3 H7C_3 109.5 . . ?
C4_3 C8_3 H8A_3 109.5 . . ?
C4_3 C8_3 H8B_3 109.5 . . ?
C4_3 C8_3 H8C_3 109.5 . . ?
H8A_3 C8_3 H8B_3 109.5 . . ?
H8A_3 C8_3 H8C_3 109.5 . . ?
H8B_3 C8_3 H8C_3 109.5 . . ?
C6_3 C9_3 H9A_3 109.5 . . ?
C6_3 C9_3 H9B_3 109.5 . . ?
C6_3 C9_3 H9C_3 109.5 . . ?
H9A_3 C9_3 H9B_3 109.5 . . ?
H9A_3 C9_3 H9C_3 109.5 . . ?
H9B_3 C9_3 H9C_3 109.5 . . ?
C2_1 C1_1 B1 112.4(9) . . ?
C6_1 C1_1 B1 122.5(10) . . ?
C6_1 C1_1 C2_1 124.8(11) . . ?
C1_1 C2_1 C3_1 113.6(10) . . ?
C1_1 C2_1 C7_1 122.8(14) . . ?
C3_1 C2_1 C7_1 123.3(14) . . ?
C2_1 C3_1 Br3 111.4(8) . . ?
C4_1 C3_1 Br3 122.3(10) . . ?
C4_1 C3_1 C2_1 126.2(11) . . ?
C3_1 C4_1 C5_1 116.6(11) . . ?
C3_1 C4_1 C8_1 124.1(14) . . ?
C5_1 C4_1 C8_1 119.3(13) . . ?
C4_1 C5_1 H5_1 119.2 . . ?
C4_1 C5_1 C6_1 121.6(12) . . ?
C6_1 C5_1 H5_1 119.2 . . ?
C1_1 C6_1 C5_1 116.5(11) . . ?
C1_1 C6_1 C9_1 121.6(13) . . ?
C5_1 C6_1 C9_1 121.9(13) . . ?
C2_1 C7_1 H7A_1 109.5 . . ?
C2_1 C7_1 H7B_1 109.5 . . ?
C2_1 C7_1 H7C_1 109.5 . . ?
H7A_1 C7_1 H7B_1 109.5 . . ?
H7A_1 C7_1 H7C_1 109.5 . . ?
H7B_1 C7_1 H7C_1 109.5 . . ?
C4_1 C8_1 H8A_1 110.2 . . ?
C4_1 C8_1 H8B_1 106.7 . . ?
C4_1 C8_1 H8C_1 111.5 . . ?
H8A_1 C8_1 H8B_1 109.5 . . ?
H8A_1 C8_1 H8C_1 109.5 . . ?
H8B_1 C8_1 H8C_1 109.5 . . ?
C6_1 C9_1 H9A_1 109.5 . . ?
C6_1 C9_1 H9B_1 109.5 . . ?
C6_1 C9_1 H9C_1 109.5 . . ?
H9A_1 C9_1 H9B_1 109.5 . . ?
H9A_1 C9_1 H9C_1 109.5 . . ?
H9B_1 C9_1 H9C_1 109.5 . . ?

_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 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.773
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
####################################################################### 
# 
# 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_lmji7
_database_code_depnum_ccdc_archive 'CCDC 1848232'
_audit_update_record             
;
2018-06-08 deposited with the CCDC.
2018-07-31 downloaded from the CCDC.
;
_audit_creation_date             2018-06-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C58 H45.87 B2 Br0.13'
_chemical_formula_sum            'C58 H45.87 B2 Br0.13'
_chemical_formula_weight         774.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H40B2
_chemical_oxdiff_usercomment     'Rachel crystal'
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'
B B 0.0090 0.0039 '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'

_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                   17.5450(17)
_cell_length_b                   12.6207(12)
_cell_length_c                   22.2518(14)
_cell_angle_alpha                90
_cell_angle_beta                 94.451(9)
_cell_angle_gamma                90
_cell_volume                     4912.4(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1822
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      62.3280
_cell_measurement_theta_min      3.9440
_shelx_estimated_absorpt_T_max   0.996
_shelx_estimated_absorpt_T_min   0.915
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.7b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1634
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.007
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1607
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        54.239
_diffrn_reflns_theta_max         54.239
_diffrn_reflns_theta_min         2.526
_diffrn_ambient_temperature      150.0(2)
_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     54.00  82.00   1.00    3.00    --    0.00  60.00-120.00   28
  2  ω    -63.00 -19.00   1.00    3.00    --    0.00  60.00-120.00   44
  3  ω    -88.00  57.00   1.00    3.00    --    0.00  60.00 -60.00  145
  4  ω      9.00  35.00   1.00    3.00    --    0.00  60.00-120.00   26
  5  ω     67.00 143.00   1.00   20.00    --   55.00  60.00   0.00   76
  6  ω    -31.00 132.00   1.00   20.00    --   55.00  57.00 -90.00  163
  7  ω     47.00 144.00   1.00   20.00    --   55.00  60.00-150.00   97
  8  ω    -31.00  46.00   1.00   20.00    --   55.00  60.00-150.00   77
  9  ω    -26.00  65.00   1.00   20.00    --   55.00  60.00   0.00   91
 10  ω     -9.00 123.00   1.00   20.00    --   55.00  60.00  90.00  132
 11  ω     87.00 138.00   1.00   20.00    --   55.00  60.00 150.00   51
 12  ω    -21.00 140.00   1.00   20.00    --   55.00  60.00  60.00  161
 13  ω     97.00 199.00   1.00   20.00    --  110.00  60.00  90.00  102
 14  ω    174.00 199.00   1.00   20.00    --  110.00  48.00  30.00   25
 15  ω     21.00 117.00   1.00   20.00    --  110.00  60.00  30.00   96
 16  ω     77.00 104.00   1.00   20.00    --  110.00  48.00  30.00   27
 17  ω     21.00  55.00   1.00   20.00    --  110.00  48.00  30.00   34
 18  ω    132.00 198.00   1.00   20.00    --  110.00  60.00 120.00   66
 19  ω     34.00 198.00   1.00   20.00    --  110.00  29.00  60.00  164
 20  ω     83.00 121.00   1.00   20.00    --  110.00  60.00 120.00   38
 21  ω     22.00 171.00   1.00   20.00    --  110.00  60.00 -60.00  149
 22  ω    125.00 197.00   1.00   20.00    --  110.00  60.00-120.00   72
 23  ω    139.00 197.00   1.00   20.00    --  110.00  60.00-180.00   58
 24  ω     57.00 122.00   1.00   20.00    --  110.00  60.00-120.00   65
 25  ω    156.00 198.00   1.00   20.00    --  110.00  60.00 150.00   42
 26  ω    132.00 159.00   1.00   20.00    --  110.00  48.00  30.00   27
 27  ω     90.00 119.00   1.00   20.00    --  110.00  60.00-180.00   29
 28  ω     22.00 176.00   1.00   20.00    --  110.00  38.00-120.00  154
 29  ω    133.00 163.00   1.00   20.00    --  110.00  60.00 -90.00   30
 30  ω     46.00  80.00   1.00   20.00    --  110.00  60.00 -30.00   34
 31  ω     32.00  59.00   1.00   20.00    --  110.00  60.00-180.00   27
 32  ω     45.00  72.00   1.00   20.00    --  110.00  60.00 -90.00   27
 33  ω    139.00 179.00   1.00   20.00    --  110.00  60.00 -30.00   40
 34  ω     83.00 115.00   1.00   20.00    --  110.00  60.00 -30.00   32
 35  ω    127.00 182.00   1.00   20.00    --  110.00  60.00  30.00   55
 36  ω     51.00  76.00   1.00   20.00    --  110.00  60.00   0.00   25
 37  ω    135.00 165.00   1.00   20.00    --  110.00  60.00   0.00   30
 38  ω     99.00 141.00   1.00   20.00    --  110.00  60.00 150.00   42
 39  ω     43.00 199.00   1.00   20.00    --  110.00  29.00 -30.00  156
 40  ω     22.00 120.00   1.00   20.00    --  110.00  19.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0075871000
_diffrn_orient_matrix_UB_12      0.0606368000
_diffrn_orient_matrix_UB_13      -0.0602439000
_diffrn_orient_matrix_UB_21      -0.0093257000
_diffrn_orient_matrix_UB_22      -0.1056965000
_diffrn_orient_matrix_UB_23      -0.0343351000
_diffrn_orient_matrix_UB_31      -0.0873064000
_diffrn_orient_matrix_UB_32      0.0059985000
_diffrn_orient_matrix_UB_33      0.0035035000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2546
_reflns_number_total             5986
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.7b (Rigaku OD, 2018)'
_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         0.410
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         5986
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1672
_refine_ls_R_factor_gt           0.0816
_refine_ls_restrained_S_all      0.979
_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)+(0.1434P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2687
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Br1-C43
 1.9 with sigma of 0.02
 Br2-C54
 1.9 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Br1, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Br1)=1-FVAR(1)
 Sof(H43)=FVAR(1)
 Sof(Br2)=1-FVAR(2)
 Sof(H54)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B)
5.b Me refined with riding coordinates:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C)
5.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C26(H26), C20(H20), C27(H27), C32(H32), C38(H38), C28(H28),
 C54(H54), C34(H34), C33(H33), C52(H52), C36(H36), C13(H13), C37(H37), C16(H16),
  C43(H43), C2(H2), C3(H3), C5(H5), C14(H14), C4(H4), C15(H15), C1(H1), C45(H45)
;
_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
C21 C 0.7063(3) 0.3160(5) 0.3471(2) 0.0725(17) Uani 1 1 d . . . . .
C25 C 0.6827(3) 0.2626(5) 0.2399(2) 0.0722(17) Uani 1 1 d . . . . .
C31 C 0.5167(3) 0.5151(5) 0.2046(3) 0.0736(17) Uani 1 1 d . . . . .
C50 C 0.5069(3) 0.5335(5) 0.3273(2) 0.0753(17) Uani 1 1 d . . . . .
C30 C 0.7185(3) 0.2455(5) 0.2989(2) 0.0707(16) Uani 1 1 d . . . . .
C22 C 0.6460(4) 0.3843(5) 0.3353(2) 0.0799(18) Uani 1 1 d . . . . .
H22 H 0.626431 0.418631 0.368846 0.096 Uiso 1 1 calc R . . . .
C24 C 0.6376(3) 0.3560(5) 0.2289(2) 0.0731(17) Uani 1 1 d . . . . .
C40 C 0.5597(3) 0.4770(5) 0.1578(2) 0.0739(17) Uani 1 1 d . . . . .
C26 C 0.6856(3) 0.1779(5) 0.1976(3) 0.0802(18) Uani 1 1 d . . . . .
H26 H 0.658502 0.185560 0.159153 0.096 Uiso 1 1 calc R . . . .
C20 C 0.8153(3) 0.1995(6) 0.4839(3) 0.0797(18) Uani 1 1 d . . . . .
H20 H 0.837882 0.133405 0.495439 0.096 Uiso 1 1 calc R . . . .
C51 C 0.4565(4) 0.4736(5) 0.3588(3) 0.0769(17) Uani 1 1 d . . . . .
C35 C 0.5466(4) 0.5211(5) 0.0988(2) 0.0824(18) Uani 1 1 d . . . . .
C39 C 0.6193(3) 0.4004(5) 0.1684(2) 0.0750(17) Uani 1 1 d . . . . .
C27 C 0.7248(3) 0.0877(6) 0.2094(2) 0.0806(18) Uani 1 1 d . . . . .
H27 H 0.725721 0.033356 0.179967 0.097 Uiso 1 1 calc R . . . .
C23 C 0.6106(3) 0.4080(5) 0.2781(2) 0.0734(17) Uani 1 1 d . . . . .
C19 C 0.7845(3) 0.2137(5) 0.4226(2) 0.0720(17) Uani 1 1 d . . . . .
C11 C 0.8131(3) 0.2776(6) 0.5257(3) 0.083(2) Uani 1 1 d . . . . .
C32 C 0.4589(3) 0.5882(5) 0.1905(2) 0.0803(18) Uani 1 1 d . . . . .
H32 H 0.429536 0.613138 0.221704 0.096 Uiso 1 1 calc R . . . .
C55 C 0.5287(4) 0.6347(6) 0.3500(3) 0.0837(19) Uani 1 1 d . . . . .
C18 C 0.7490(3) 0.3087(5) 0.4064(2) 0.0710(17) Uani 1 1 d . . . . .
C53 C 0.4536(4) 0.6078(6) 0.4364(3) 0.0849(19) Uani 1 1 d . . . . .
C38 C 0.6651(4) 0.3795(5) 0.1215(2) 0.0861(19) Uani 1 1 d . . . . .
H38 H 0.707283 0.332786 0.128926 0.103 Uiso 1 1 calc R . . . .
C28 C 0.7641(3) 0.0756(5) 0.2659(3) 0.0818(18) Uani 1 1 d . . . . .
H28 H 0.794543 0.014081 0.273525 0.098 Uiso 1 1 calc R . . . .
C54 C 0.5016(4) 0.6690(6) 0.4050(3) 0.088(2) Uani 1 1 d D . . . .
H54 H 0.516985 0.736409 0.420587 0.105 Uiso 0.915(3) 1 calc R . P A 2
C34 C 0.4867(4) 0.5954(5) 0.0886(3) 0.087(2) Uani 1 1 d . . . . .
H34 H 0.477142 0.624910 0.049441 0.105 Uiso 1 1 calc R . . . .
C41 C 0.8394(4) 0.0209(6) 0.3939(3) 0.0853(19) Uani 1 1 d . . . . .
C33 C 0.4428(4) 0.6258(6) 0.1324(3) 0.090(2) Uani 1 1 d . . . . .
H33 H 0.401093 0.672768 0.123604 0.108 Uiso 1 1 calc R . . . .
C29 C 0.7606(3) 0.1491(5) 0.3109(2) 0.0731(17) Uani 1 1 d . . . . .
C52 C 0.4317(4) 0.5124(6) 0.4119(3) 0.088(2) Uani 1 1 d . . . . .
H52 H 0.397364 0.470140 0.432678 0.106 Uiso 1 1 calc R . . B 2
C12 C 0.7847(3) 0.3784(6) 0.5086(3) 0.0813(19) Uani 1 1 d . . . . .
C17 C 0.7544(3) 0.3970(6) 0.4471(2) 0.0825(19) Uani 1 1 d . . . . .
C42 C 0.9206(4) 0.0194(6) 0.4001(3) 0.092(2) Uani 1 1 d . . . . .
C36 C 0.5945(4) 0.4918(6) 0.0532(3) 0.093(2) Uani 1 1 d . . . . .
H36 H 0.585338 0.521226 0.013977 0.111 Uiso 1 1 calc R . . . .
C13 C 0.7844(4) 0.4647(7) 0.5499(3) 0.098(2) Uani 1 1 d . . . . .
H13 H 0.801099 0.453219 0.591045 0.118 Uiso 1 1 calc R . . . .
C10 C 0.8424(3) 0.2592(6) 0.5874(3) 0.087(2) Uani 1 1 d . . . . .
C37 C 0.6524(4) 0.4236(6) 0.0639(2) 0.093(2) Uani 1 1 d . . . . .
H37 H 0.684341 0.405416 0.032929 0.112 Uiso 1 1 calc R . . . .
C9 C 0.8689(4) 0.2442(6) 0.6371(3) 0.097(2) Uani 1 1 d . . . . .
C6 C 0.9397(5) 0.0812(6) 0.7742(3) 0.103(2) Uani 1 1 d . . . . .
C56 C 0.4295(4) 0.3668(6) 0.3346(3) 0.104(2) Uani 1 1 d . . . . .
H56A H 0.452765 0.352234 0.296784 0.155 Uiso 1 1 calc R . . . .
H56B H 0.444610 0.311605 0.364111 0.155 Uiso 1 1 calc R . . . .
H56C H 0.373734 0.367447 0.327138 0.155 Uiso 1 1 calc R . . . .
C57 C 0.4256(4) 0.6453(6) 0.4955(2) 0.106(2) Uani 1 1 d . . . . .
H57A H 0.447352 0.715172 0.505558 0.159 Uiso 1 1 calc R . . . .
H57B H 0.369651 0.650232 0.491585 0.159 Uiso 1 1 calc R . . . .
H57C H 0.441564 0.594859 0.527456 0.159 Uiso 1 1 calc R . . . .
C16 C 0.7368(4) 0.5053(6) 0.4312(3) 0.098(2) Uani 1 1 d . . . . .
H16 H 0.723611 0.521973 0.390065 0.118 Uiso 1 1 calc R . . . .
C43 C 0.9588(4) -0.0754(8) 0.4207(3) 0.106(2) Uani 1 1 d D U . . .
H43 H 1.013072 -0.077496 0.424034 0.128 Uiso 0.956(3) 1 calc R . P C 2
C8 C 0.9047(4) 0.2210(7) 0.6985(3) 0.114(3) Uani 1 1 d . . . . .
H8A H 0.880832 0.265876 0.728301 0.137 Uiso 1 1 calc R . . . .
H8B H 0.959849 0.238385 0.700202 0.137 Uiso 1 1 calc R . . . .
C2 C 0.9492(5) 0.0760(7) 0.8822(3) 0.114(3) Uani 1 1 d . . . . .
H2 H 0.927405 0.092336 0.918831 0.137 Uiso 1 1 calc R . . . .
C44 C 0.9188(5) -0.1627(8) 0.4355(3) 0.115(3) Uani 1 1 d . . . . .
B2 B 0.5438(4) 0.4885(6) 0.2705(3) 0.074(2) Uani 1 1 d . . . . .
C46 C 0.8004(4) -0.0691(7) 0.4089(3) 0.103(2) Uani 1 1 d . . . . .
C3 C 1.0172(5) 0.0286(7) 0.8833(3) 0.112(3) Uani 1 1 d . . . . .
H3 H 1.043542 0.009294 0.920601 0.135 Uiso 1 1 calc R . . . .
C58 C 0.5826(4) 0.7054(6) 0.3178(3) 0.115(3) Uani 1 1 d . . . . .
H58A H 0.590772 0.771711 0.340235 0.172 Uiso 1 1 calc R . . . .
H58B H 0.631612 0.669096 0.315270 0.172 Uiso 1 1 calc R . . . .
H58C H 0.560075 0.720916 0.277037 0.172 Uiso 1 1 calc R . . . .
C5 C 1.0098(5) 0.0345(7) 0.7762(3) 0.128(3) Uani 1 1 d . . . . .
H5 H 1.032131 0.020029 0.739545 0.154 Uiso 1 1 calc R . . . .
C7 C 0.8950(5) 0.1074(7) 0.7140(3) 0.121(3) Uani 1 1 d . . . . .
H7A H 0.913559 0.062360 0.681769 0.145 Uiso 1 1 calc R . . . .
H7B H 0.840109 0.091917 0.716947 0.145 Uiso 1 1 calc R . . . .
B1 B 0.7948(4) 0.1269(6) 0.3758(3) 0.075(2) Uani 1 1 d . . . . .
C14 C 0.7608(4) 0.5627(7) 0.5320(3) 0.112(3) Uani 1 1 d . . . . .
H14 H 0.759509 0.617727 0.561040 0.135 Uiso 1 1 calc R . . . .
C4 C 1.0489(5) 0.0079(7) 0.8297(4) 0.125(3) Uani 1 1 d . . . . .
H4 H 1.097680 -0.024807 0.829914 0.150 Uiso 1 1 calc R . . . .
C15 C 0.7384(4) 0.5843(6) 0.4722(3) 0.114(3) Uani 1 1 d . . . . .
H15 H 0.724251 0.654248 0.460079 0.137 Uiso 1 1 calc R . . . .
C47 C 0.9643(4) 0.1150(7) 0.3834(3) 0.117(3) Uani 1 1 d . . . . .
H47A H 1.019197 0.101089 0.390342 0.175 Uiso 1 1 calc R . . . .
H47B H 0.951797 0.131513 0.340749 0.175 Uiso 1 1 calc R . . . .
H47C H 0.950474 0.175232 0.408169 0.175 Uiso 1 1 calc R . . . .
C1 C 0.9103(4) 0.1014(7) 0.8276(3) 0.128(3) Uani 1 1 d . . . . .
H1 H 0.861471 0.133899 0.827540 0.153 Uiso 1 1 calc R . . . .
C45 C 0.8386(5) -0.1625(8) 0.4295(4) 0.138(3) Uani 1 1 d . . . . .
H45 H 0.810528 -0.223781 0.438985 0.165 Uiso 1 1 calc R . . D 2
C49 C 0.7124(4) -0.0690(7) 0.4053(4) 0.133(3) Uani 1 1 d . . . . .
H49A H 0.694103 -0.138562 0.417423 0.199 Uiso 1 1 calc R . . . .
H49B H 0.694660 -0.014500 0.432321 0.199 Uiso 1 1 calc R . . . .
H49C H 0.692427 -0.053825 0.363833 0.199 Uiso 1 1 calc R . . . .
C48 C 0.9607(5) -0.2626(7) 0.4588(4) 0.153(4) Uani 1 1 d . . . . .
H48A H 0.923283 -0.317235 0.467157 0.230 Uiso 1 1 calc R . . . .
H48B H 0.993379 -0.288580 0.428180 0.230 Uiso 1 1 calc R . . . .
H48C H 0.992233 -0.245906 0.495828 0.230 Uiso 1 1 calc R . . . .
Br2 Br 0.5472(5) 0.7783(8) 0.4441(4) 0.111(5) Uani 0.085(3) 1 d D . P A 1
Br1 Br 1.0637(9) -0.0291(16) 0.4247(8) 0.126(12) Uani 0.044(3) 1 d D U P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C21 C30 1.422(7) . ?
C21 C22 1.374(8) . ?
C21 C18 1.471(7) . ?
C25 C30 1.427(7) . ?
C25 C24 1.430(8) . ?
C25 C26 1.429(8) . ?
C31 C40 1.415(8) . ?
C31 C32 1.388(8) . ?
C31 B2 1.544(8) . ?
C50 C51 1.393(8) . ?
C50 C55 1.415(8) . ?
C50 B2 1.571(9) . ?
C30 C29 1.438(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.403(7) . ?
C24 C39 1.470(7) . ?
C24 C23 1.391(7) . ?
C40 C35 1.429(7) . ?
C40 C39 1.430(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.346(8) . ?
C20 H20 0.9500 . ?
C20 C19 1.438(7) . ?
C20 C11 1.358(8) . ?
C51 C52 1.381(8) . ?
C51 C56 1.513(8) . ?
C35 C34 1.414(8) . ?
C35 C36 1.417(8) . ?
C39 C38 1.393(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.395(7) . ?
C23 B2 1.551(9) . ?
C19 C18 1.385(8) . ?
C19 B1 1.532(9) . ?
C11 C12 1.408(8) . ?
C11 C10 1.447(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.386(7) . ?
C55 C54 1.415(8) . ?
C55 C58 1.519(8) . ?
C18 C17 1.434(8) . ?
C53 C54 1.374(8) . ?
C53 C52 1.364(8) . ?
C53 C57 1.515(8) . ?
C38 H38 0.9500 . ?
C38 C37 1.398(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.369(8) . ?
C54 H54 0.9500 . ?
C54 Br2 1.787(10) . ?
C34 H34 0.9500 . ?
C34 C33 1.344(8) . ?
C41 C42 1.422(9) . ?
C41 C46 1.380(9) . ?
C41 B1 1.586(10) . ?
C33 H33 0.9500 . ?
C29 B1 1.545(8) . ?
C52 H52 0.9500 . ?
C12 C17 1.449(8) . ?
C12 C13 1.426(8) . ?
C17 C16 1.439(9) . ?
C42 C43 1.428(10) . ?
C42 C47 1.492(9) . ?
C36 H36 0.9500 . ?
C36 C37 1.339(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.354(9) . ?
C10 C9 1.181(7) . ?
C37 H37 0.9500 . ?
C9 C8 1.488(8) . ?
C6 C5 1.361(9) . ?
C6 C7 1.534(8) . ?
C6 C1 1.356(9) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C16 H16 0.9500 . ?
C16 C15 1.350(8) . ?
C43 H43 0.9500 . ?
C43 C44 1.361(10) . ?
C43 Br1 1.927(16) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.488(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.334(9) . ?
C2 C1 1.383(8) . ?
C44 C45 1.403(10) . ?
C44 C48 1.528(10) . ?
C46 C45 1.414(10) . ?
C46 C49 1.540(9) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(9) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C5 H5 0.9500 . ?
C5 C4 1.369(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C14 H14 0.9500 . ?
C14 C15 1.386(9) . ?
C4 H4 0.9500 . ?
C15 H15 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C1 H1 0.9500 . ?
C45 H45 0.9500 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C30 C21 C18 122.8(6) . . ?
C22 C21 C30 114.0(5) . . ?
C22 C21 C18 122.9(6) . . ?
C30 C25 C24 118.7(6) . . ?
C30 C25 C26 117.2(6) . . ?
C26 C25 C24 123.4(5) . . ?
C40 C31 B2 118.9(6) . . ?
C32 C31 C40 118.8(5) . . ?
C32 C31 B2 121.6(6) . . ?
C51 C50 C55 118.4(6) . . ?
C51 C50 B2 121.7(6) . . ?
C55 C50 B2 119.7(6) . . ?
C21 C30 C25 121.2(6) . . ?
C21 C30 C29 119.7(5) . . ?
C25 C30 C29 118.8(6) . . ?
C21 C22 H22 117.1 . . ?
C21 C22 C23 125.9(6) . . ?
C23 C22 H22 117.1 . . ?
C25 C24 C39 123.3(5) . . ?
C23 C24 C25 118.1(5) . . ?
C23 C24 C39 118.5(6) . . ?
C31 C40 C35 119.1(6) . . ?
C31 C40 C39 122.2(5) . . ?
C35 C40 C39 118.6(5) . . ?
C25 C26 H26 118.4 . . ?
C27 C26 C25 123.2(6) . . ?
C27 C26 H26 118.4 . . ?
C19 C20 H20 119.0 . . ?
C11 C20 H20 119.0 . . ?
C11 C20 C19 122.0(6) . . ?
C50 C51 C56 119.8(6) . . ?
C52 C51 C50 119.5(6) . . ?
C52 C51 C56 120.7(6) . . ?
C34 C35 C40 118.1(6) . . ?
C34 C35 C36 122.2(6) . . ?
C36 C35 C40 119.7(6) . . ?
C40 C39 C24 120.9(5) . . ?
C38 C39 C24 121.1(6) . . ?
C38 C39 C40 117.5(5) . . ?
C26 C27 H27 120.7 . . ?
C26 C27 C28 118.6(6) . . ?
C28 C27 H27 120.7 . . ?
C22 C23 B2 121.0(5) . . ?
C24 C23 C22 117.4(6) . . ?
C24 C23 B2 121.6(5) . . ?
C20 C19 B1 120.0(6) . . ?
C18 C19 C20 118.9(6) . . ?
C18 C19 B1 121.0(5) . . ?
C20 C11 C12 120.0(5) . . ?
C20 C11 C10 120.4(7) . . ?
C12 C11 C10 119.6(6) . . ?
C31 C32 H32 119.0 . . ?
C33 C32 C31 122.0(6) . . ?
C33 C32 H32 119.0 . . ?
C50 C55 C54 119.0(6) . . ?
C50 C55 C58 121.6(6) . . ?
C54 C55 C58 119.4(7) . . ?
C19 C18 C21 118.4(6) . . ?
C19 C18 C17 120.2(5) . . ?
C17 C18 C21 121.4(6) . . ?
C54 C53 C57 121.2(7) . . ?
C52 C53 C54 117.3(6) . . ?
C52 C53 C57 121.5(7) . . ?
C39 C38 H38 118.3 . . ?
C39 C38 C37 123.4(6) . . ?
C37 C38 H38 118.3 . . ?
C27 C28 H28 118.7 . . ?
C29 C28 C27 122.5(6) . . ?
C29 C28 H28 118.7 . . ?
C55 C54 H54 119.1 . . ?
C55 C54 Br2 119.3(6) . . ?
C53 C54 C55 121.9(7) . . ?
C53 C54 H54 119.1 . . ?
C53 C54 Br2 117.1(6) . . ?
C35 C34 H34 118.9 . . ?
C33 C34 C35 122.2(6) . . ?
C33 C34 H34 118.9 . . ?
C42 C41 B1 120.5(7) . . ?
C46 C41 C42 118.4(7) . . ?
C46 C41 B1 120.8(6) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 C32 119.5(6) . . ?
C34 C33 H33 120.3 . . ?
C30 C29 B1 118.9(6) . . ?
C28 C29 C30 119.3(5) . . ?
C28 C29 B1 121.6(6) . . ?
C51 C52 H52 118.1 . . ?
C53 C52 C51 123.8(7) . . ?
C53 C52 H52 118.1 . . ?
C11 C12 C17 119.8(6) . . ?
C11 C12 C13 122.4(6) . . ?
C13 C12 C17 117.8(7) . . ?
C18 C17 C12 118.1(6) . . ?
C18 C17 C16 125.6(6) . . ?
C16 C17 C12 116.2(6) . . ?
C41 C42 C43 119.0(7) . . ?
C41 C42 C47 119.6(7) . . ?
C43 C42 C47 121.3(7) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.6(6) . . ?
C37 C36 H36 119.2 . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.6(7) . . ?
C14 C13 H13 119.2 . . ?
C9 C10 C11 177.7(7) . . ?
C38 C37 H37 120.5 . . ?
C36 C37 C38 119.0(6) . . ?
C36 C37 H37 120.5 . . ?
C10 C9 C8 177.2(8) . . ?
C5 C6 C7 121.4(7) . . ?
C1 C6 C5 117.2(7) . . ?
C1 C6 C7 121.4(7) . . ?
C51 C56 H56A 109.5 . . ?
C51 C56 H56B 109.5 . . ?
C51 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C53 C57 H57A 109.5 . . ?
C53 C57 H57B 109.5 . . ?
C53 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C17 C16 H16 118.6 . . ?
C15 C16 C17 122.9(7) . . ?
C15 C16 H16 118.6 . . ?
C42 C43 H43 119.4 . . ?
C42 C43 Br1 100.6(9) . . ?
C44 C43 C42 121.2(8) . . ?
C44 C43 H43 119.4 . . ?
C44 C43 Br1 138.0(9) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C9 C8 C7 110.8(6) . . ?
H8A C8 H8B 108.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C3 C2 H2 120.0 . . ?
C3 C2 C1 120.0(7) . . ?
C1 C2 H2 120.0 . . ?
C43 C44 C45 120.5(8) . . ?
C43 C44 C48 120.4(8) . . ?
C45 C44 C48 119.1(9) . . ?
C31 B2 C50 124.8(6) . . ?
C31 B2 C23 114.8(5) . . ?
C23 B2 C50 120.3(5) . . ?
C41 C46 C45 122.2(8) . . ?
C41 C46 C49 120.0(7) . . ?
C45 C46 C49 117.7(8) . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.3(7) . . ?
C4 C3 H3 120.4 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C6 C5 H5 119.1 . . ?
C6 C5 C4 121.7(7) . . ?
C4 C5 H5 119.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 C6 110.5(7) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C19 B1 C41 120.8(5) . . ?
C19 B1 C29 116.7(6) . . ?
C29 B1 C41 122.5(6) . . ?
C13 C14 H14 119.3 . . ?
C13 C14 C15 121.4(8) . . ?
C15 C14 H14 119.3 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.8(7) . . ?
C5 C4 H4 120.1 . . ?
C16 C15 C14 119.5(8) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C6 C1 C2 122.0(7) . . ?
C6 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C44 C45 C46 118.7(9) . . ?
C44 C45 H45 120.7 . . ?
C46 C45 H45 120.7 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

_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 0.203 0.201 0.304 230.5 50.4 ?
2 0.203 0.299 0.804 230.5 50.4 ?
3 -0.203 0.701 0.196 230.5 50.3 ?
4 -0.203 0.799 0.696 230.5 50.4 ?

_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 4.356
_oxdiff_exptl_absorpt_empirical_full_min 0.392
_vrf_THETM01_lmji7               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystals of the sample are very weakly diffracting, therefore the 
data were truncated accordingly. Despite best efforts, better data could not 
be obtained using a synchrotron source
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
