# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_3RD_AORIG_SQ
_database_code_depnum_ccdc_archive 'CCDC 1436391'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;


#======================================================================
# start Validation Reply Form


_vrf_EXPT009_I                   
;
PROBLEM:  No crystal dimensions have been given.  The following tests 
will not be performed.  CRYSS_01,CRYSS_02
RESPONSE: Crystal was dismounted before collecting video for crystal
dimensions.  No other crystals are available.
;

_vrf_EXPT108_I                   
;
PROBLEM: The magnitudes of the crystal dimensions do not
match the min, mid and max definitions
RESPONSE:  No crystal dimensions were taken.
;
# end Validation Reply Form



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C61 H62 B2 N2, 2(C Cl2)'
_chemical_formula_sum            'C63 H62 B2 Cl4 N2'
_chemical_formula_weight         1010.56

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   15.19(1)
_cell_length_b                   17.546(12)
_cell_length_c                   20.226(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5391(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9985
_cell_measurement_theta_min      3.34
_cell_measurement_theta_max      69.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_F_000             2128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.307
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47791
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.334
_diffrn_reflns_theta_max         70.162
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8930
_reflns_number_gt                8175
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_max     0.972
_reflns_Friedel_fraction_full    0.998

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          'DCM solvent molecules show disorder'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1333P)²+5.8594P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8930
_refine_ls_number_parameters     665
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2102
_refine_ls_wR_factor_gt          0.2023
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
B1 B 0.1669(4) 0.5226(3) 0.5618(3) 0.0189(11) Uani 1 1 d . . . . .
B2 B 0.6371(4) 0.3839(3) 0.3648(3) 0.0212(12) Uani 1 1 d . . . . .
Cl4 Cl 0.7226(3) 0.1265(2) 0.24099(17) 0.1190(14) Uani 1 1 d D . . . .
Cl3 Cl 0.8420(2) 0.0331(3) 0.3161(4) 0.150(2) Uani 1 1 d D . . . .
N1 N 0.1186(3) 0.5019(2) 0.6323(2) 0.0207(9) Uani 1 1 d . . . . .
N2 N 0.7095(3) 0.3168(2) 0.3778(2) 0.0193(9) Uani 1 1 d . . . . .
C1 C 0.2537(3) 0.4719(3) 0.5737(3) 0.0179(10) Uani 1 1 d . . . . .
C2 C 0.3262(3) 0.4600(3) 0.5323(3) 0.0180(10) Uani 1 1 d . . . . .
H2 H 0.3316 0.4871 0.4918 0.022 Uiso 1 1 calc R U . . .
C3 C 0.3906(3) 0.4074(3) 0.5516(3) 0.0185(10) Uani 1 1 d . . . . .
C4 C 0.3841(3) 0.3668(3) 0.6112(3) 0.0185(10) Uani 1 1 d . . . . .
C5 C 0.3144(3) 0.3801(3) 0.6545(3) 0.0197(10) Uani 1 1 d . . . . .
H5 H 0.3107 0.3550 0.6960 0.024 Uiso 1 1 calc R U . . .
C6 C 0.2498(3) 0.4326(3) 0.6339(3) 0.0190(10) Uani 1 1 d . . . . .
C7 C 0.1691(3) 0.4532(3) 0.6695(3) 0.0215(11) Uani 1 1 d . . . . .
C8 C 0.1429(4) 0.4311(3) 0.7327(3) 0.0250(12) Uani 1 1 d . . . . .
H8 H 0.1789 0.3985 0.7586 0.030 Uiso 1 1 calc R U . . .
C9 C 0.0628(4) 0.4578(3) 0.7569(3) 0.0283(12) Uani 1 1 d . . . . .
H9 H 0.0432 0.4436 0.7998 0.034 Uiso 1 1 calc R U . . .
C10 C 0.0119(4) 0.5056(3) 0.7177(3) 0.0264(12) Uani 1 1 d . . . . .
H10 H -0.0433 0.5230 0.7336 0.032 Uiso 1 1 calc R U . . .
C11 C 0.0403(4) 0.5282(3) 0.6557(3) 0.0227(11) Uani 1 1 d . . . . .
C12 C -0.0130(4) 0.5811(3) 0.6131(3) 0.0265(12) Uani 1 1 d . . . . .
H12A H -0.0692 0.5921 0.6349 0.040 Uiso 1 1 calc R U . . .
H12B H -0.0240 0.5569 0.5702 0.040 Uiso 1 1 calc R U . . .
H12C H 0.0195 0.6287 0.6064 0.040 Uiso 1 1 calc R U . . .
C13 C 0.1869(3) 0.6138(3) 0.5611(3) 0.0197(10) Uani 1 1 d . . . . .
C14 C 0.2473(4) 0.6432(3) 0.6072(3) 0.0271(12) Uani 1 1 d . . . . .
H14 H 0.2759 0.6093 0.6369 0.033 Uiso 1 1 calc R U . . .
C15 C 0.2660(4) 0.7202(4) 0.6104(4) 0.0372(15) Uani 1 1 d . . . . .
H15 H 0.3062 0.7383 0.6428 0.045 Uiso 1 1 calc R U . . .
C16 C 0.2272(4) 0.7713(3) 0.5672(4) 0.0358(14) Uani 1 1 d . . . . .
H16 H 0.2417 0.8239 0.5686 0.043 Uiso 1 1 calc R U . . .
C17 C 0.1662(4) 0.7437(3) 0.5212(3) 0.0316(13) Uani 1 1 d . . . . .
H17 H 0.1379 0.7778 0.4917 0.038 Uiso 1 1 calc R U . . .
C18 C 0.1471(4) 0.6667(3) 0.5189(3) 0.0258(12) Uani 1 1 d . . . . .
H18 H 0.1054 0.6491 0.4874 0.031 Uiso 1 1 calc R U . . .
C19 C 0.1134(3) 0.4867(3) 0.5004(3) 0.0176(10) Uani 1 1 d . . . . .
C20 C 0.0477(4) 0.4302(3) 0.5061(3) 0.0247(11) Uani 1 1 d . . . . .
H20 H 0.0279 0.4160 0.5490 0.030 Uiso 1 1 calc R U . . .
C21 C 0.0108(4) 0.3946(3) 0.4510(3) 0.0282(12) Uani 1 1 d . . . . .
H21 H -0.0333 0.3568 0.4569 0.034 Uiso 1 1 calc R U . . .
C22 C 0.0377(4) 0.4137(3) 0.3881(3) 0.0274(12) Uani 1 1 d . . . . .
H22 H 0.0120 0.3899 0.3506 0.033 Uiso 1 1 calc R U . . .
C23 C 0.1035(4) 0.4687(3) 0.3807(3) 0.0255(12) Uani 1 1 d . . . . .
H23 H 0.1235 0.4819 0.3377 0.031 Uiso 1 1 calc R U . . .
C24 C 0.1396(3) 0.5041(3) 0.4354(3) 0.0226(11) Uani 1 1 d . . . . .
H24 H 0.1838 0.5417 0.4288 0.027 Uiso 1 1 calc R U . . .
C31 C 0.5769(3) 0.3671(3) 0.4287(3) 0.0190(10) Uani 1 1 d . . . . .
C32 C 0.5033(3) 0.4041(3) 0.4551(3) 0.0188(10) Uani 1 1 d . . . . .
H32 H 0.4771 0.4454 0.4319 0.023 Uiso 1 1 calc R U . . .
C33 C 0.4685(3) 0.3806(3) 0.5157(3) 0.0181(10) Uani 1 1 d . . . . .
C34 C 0.5070(3) 0.3203(3) 0.5526(3) 0.0190(10) Uani 1 1 d . . . . .
C35 C 0.5779(3) 0.2810(3) 0.5265(3) 0.0188(10) Uani 1 1 d . . . . .
H35 H 0.6032 0.2391 0.5494 0.023 Uiso 1 1 calc R U . . .
C36 C 0.6111(3) 0.3050(3) 0.4654(3) 0.0188(10) Uani 1 1 d . . . . .
C37 C 0.6889(3) 0.2738(3) 0.4320(3) 0.0190(10) Uani 1 1 d . . . . .
C38 C 0.7387(4) 0.2105(3) 0.4500(3) 0.0250(11) Uani 1 1 d . . . . .
H38 H 0.7223 0.1795 0.4865 0.030 Uiso 1 1 calc R U . . .
C39 C 0.8124(4) 0.1946(4) 0.4130(3) 0.0307(13) Uani 1 1 d . . . . .
H39 H 0.8482 0.1522 0.4244 0.037 Uiso 1 1 calc R U . . .
C40 C 0.8351(4) 0.2395(3) 0.3595(3) 0.0281(12) Uani 1 1 d . . . . .
H40 H 0.8872 0.2289 0.3353 0.034 Uiso 1 1 calc R U . . .
C41 C 0.7814(3) 0.3003(3) 0.3412(3) 0.0233(11) Uani 1 1 d . . . . .
C42 C 0.8013(4) 0.3461(4) 0.2805(3) 0.0315(13) Uani 1 1 d . . . . .
H42A H 0.7789 0.3193 0.2414 0.047 Uiso 1 1 calc R U . . .
H42B H 0.8651 0.3527 0.2764 0.047 Uiso 1 1 calc R U . . .
H42C H 0.7730 0.3961 0.2839 0.047 Uiso 1 1 calc R U . . .
C43 C 0.6829(4) 0.4674(3) 0.3723(3) 0.0256(12) Uani 1 1 d . . . . .
C44 C 0.6303(5) 0.5330(3) 0.3616(3) 0.0348(14) Uani 1 1 d . . . . .
H44 H 0.5713 0.5267 0.3470 0.042 Uiso 1 1 calc R U . . .
C45 C 0.6623(6) 0.6062(4) 0.3719(4) 0.0471(19) Uani 1 1 d . . . . .
H45 H 0.6259 0.6490 0.3629 0.057 Uiso 1 1 calc R U . . .
C46 C 0.7479(6) 0.6170(4) 0.3956(4) 0.051(2) Uani 1 1 d . . . . .
H46 H 0.7699 0.6670 0.4032 0.061 Uiso 1 1 calc R U . . .
C47 C 0.7999(5) 0.5541(4) 0.4078(4) 0.0434(17) Uani 1 1 d . . . . .
H47 H 0.8578 0.5607 0.4245 0.052 Uiso 1 1 calc R U . . .
C48 C 0.7678(4) 0.4801(4) 0.3958(3) 0.0295(13) Uani 1 1 d . . . . .
H48 H 0.8051 0.4377 0.4039 0.035 Uiso 1 1 calc R U . . .
C49 C 0.5902(3) 0.3658(3) 0.2942(3) 0.0243(12) Uani 1 1 d . . . . .
C50 C 0.5550(4) 0.2925(4) 0.2834(3) 0.0298(13) Uani 1 1 d . . . . .
H50 H 0.5580 0.2559 0.3179 0.036 Uiso 1 1 calc R U . . .
C51 C 0.5159(4) 0.2721(5) 0.2231(3) 0.0416(16) Uani 1 1 d . . . . .
H51 H 0.4943 0.2218 0.2169 0.050 Uiso 1 1 calc R U . . .
C52 C 0.5085(4) 0.3250(5) 0.1727(3) 0.048(2) Uani 1 1 d . . . . .
H52 H 0.4803 0.3117 0.1324 0.058 Uiso 1 1 calc R U . . .
C53 C 0.5429(4) 0.3977(5) 0.1817(3) 0.0437(17) Uani 1 1 d . . . . .
H53 H 0.5390 0.4343 0.1472 0.052 Uiso 1 1 calc R U . . .
C54 C 0.5830(4) 0.4167(4) 0.2414(3) 0.0330(13) Uani 1 1 d . . . . .
H54 H 0.6065 0.4666 0.2464 0.040 Uiso 1 1 calc R U . . .
C55 C 0.4613(3) 0.3113(3) 0.6198(3) 0.0198(11) Uani 1 1 d . . . . .
C56 C 0.4325(3) 0.2291(3) 0.6346(3) 0.0214(11) Uani 1 1 d . . . . .
H56A H 0.4846 0.1956 0.6303 0.026 Uiso 1 1 calc R U . . .
H56B H 0.4127 0.2265 0.6811 0.026 Uiso 1 1 calc R U . . .
C57 C 0.3597(4) 0.1970(3) 0.5911(3) 0.0225(11) Uani 1 1 d . . . . .
H57A H 0.3778 0.2013 0.5442 0.027 Uiso 1 1 calc R U . . .
H57B H 0.3060 0.2282 0.5971 0.027 Uiso 1 1 calc R U . . .
C58 C 0.3377(4) 0.1140(3) 0.6061(3) 0.0267(12) Uani 1 1 d . . . . .
H58A H 0.3303 0.1081 0.6545 0.032 Uiso 1 1 calc R U . . .
H58B H 0.3881 0.0818 0.5926 0.032 Uiso 1 1 calc R U . . .
C59 C 0.2546(4) 0.0849(3) 0.5717(3) 0.0257(11) Uani 1 1 d . . . . .
H59A H 0.2041 0.1165 0.5858 0.031 Uiso 1 1 calc R U . . .
H59B H 0.2617 0.0913 0.5234 0.031 Uiso 1 1 calc R U . . .
C60 C 0.2341(4) 0.0020(3) 0.5862(3) 0.0309(14) Uani 1 1 d . . . . .
H60A H 0.2350 -0.0058 0.6347 0.037 Uiso 1 1 calc R U . . .
H60B H 0.2811 -0.0301 0.5668 0.037 Uiso 1 1 calc R U . . .
C61 C 0.1458(4) -0.0247(3) 0.5595(3) 0.0305(13) Uani 1 1 d . . . . .
H61A H 0.0983 0.0030 0.5818 0.046 Uiso 1 1 calc R U . . .
H61B H 0.1392 -0.0795 0.5677 0.046 Uiso 1 1 calc R U . . .
H61C H 0.1430 -0.0149 0.5119 0.046 Uiso 1 1 calc R U . . .
C62 C 0.5198(4) 0.3437(3) 0.6766(3) 0.0229(11) Uani 1 1 d . . . . .
H62A H 0.5404 0.3949 0.6631 0.027 Uiso 1 1 calc R U . . .
H3W H 0.4821 0.3505 0.7161 0.027 Uiso 1 1 calc R U . . .
C63 C 0.6002(4) 0.2969(3) 0.6970(3) 0.0245(11) Uani 1 1 d . . . . .
H63A H 0.5807 0.2497 0.7195 0.029 Uiso 1 1 calc R U . . .
H63B H 0.6340 0.2821 0.6571 0.029 Uiso 1 1 calc R U . . .
C64 C 0.6590(4) 0.3426(3) 0.7432(3) 0.0339(14) Uani 1 1 d . . . . .
H64A H 0.6778 0.3893 0.7198 0.041 Uiso 1 1 calc R U . . .
H64B H 0.6232 0.3587 0.7817 0.041 Uiso 1 1 calc R U . . .
C65 C 0.7399(4) 0.3027(3) 0.7687(3) 0.0265(12) Uani 1 1 d . . . . .
H65A H 0.7720 0.2800 0.7309 0.032 Uiso 1 1 calc R U . . .
H65B H 0.7217 0.2605 0.7982 0.032 Uiso 1 1 calc R U . . .
C66 C 0.8015(5) 0.3552(4) 0.8061(4) 0.0378(15) Uani 1 1 d . . . . .
H66A H 0.7685 0.3788 0.8430 0.045 Uiso 1 1 calc R U . . .
H66B H 0.8203 0.3967 0.7761 0.045 Uiso 1 1 calc R U . . .
C67 C 0.8831(4) 0.3170(4) 0.8341(3) 0.0354(14) Uani 1 1 d . . . . .
H67A H 0.8657 0.2792 0.8672 0.053 Uiso 1 1 calc R U . . .
H67B H 0.9210 0.3555 0.8547 0.053 Uiso 1 1 calc R U . . .
H67C H 0.9154 0.2917 0.7983 0.053 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4357(3) 0.7683(3) 0.4766(5) 0.086(3) Uani 0.563(17) 1 d D . P . .
Cl1A Cl 0.4314(5) 0.7601(6) 0.4183(9) 0.114(6) Uani 0.437(17) 1 d D . P . .
Cl2 Cl 0.4632(4) 0.6136(3) 0.4725(8) 0.109(6) Uani 0.451(16) 1 d D . P . .
Cl2A Cl 0.4164(9) 0.6166(3) 0.4165(4) 0.117(5) Uani 0.549(16) 1 d D . P . .
C70 C 0.3938(11) 0.6833(7) 0.4766(8) 0.123(5) Uani 1 1 d D . . . .
C71 C 0.8338(9) 0.0895(10) 0.2525(7) 0.116(5) Uani 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 C1 1.609(7) . ?
B1 C19 1.613(8) . ?
B1 C13 1.630(7) . ?
B1 N1 1.644(7) . ?
B2 C31 1.610(8) . ?
B2 C49 1.627(9) . ?
B2 C43 1.629(8) . ?
B2 N2 1.632(7) . ?
Cl4 C71 1.825(15) . ?
Cl3 C71 1.626(16) . ?
N1 C11 1.361(7) . ?
N1 C7 1.373(7) . ?
N2 C41 1.350(7) . ?
N2 C37 1.367(7) . ?
C1 C2 1.400(7) . ?
C1 C6 1.401(8) . ?
C2 C3 1.400(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(7) . ?
C3 C33 1.466(7) . ?
C4 C5 1.394(7) . ?
C4 C55 1.535(7) . ?
C5 C6 1.409(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.467(7) . ?
C7 C8 1.393(8) . ?
C8 C9 1.394(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.503(8) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.399(8) . ?
C13 C14 1.406(8) . ?
C14 C15 1.382(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.398(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.407(8) . ?
C19 C20 1.412(8) . ?
C20 C21 1.396(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.377(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.398(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C31 C32 1.399(7) . ?
C31 C36 1.418(7) . ?
C32 C33 1.397(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.420(7) . ?
C34 C35 1.383(7) . ?
C34 C55 1.535(7) . ?
C35 C36 1.400(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.467(7) . ?
C37 C38 1.392(8) . ?
C38 C39 1.376(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.382(9) . ?
C39 H39 0.9500 . ?
C40 C41 1.394(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.498(8) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C48 1.392(9) . ?
C43 C44 1.418(8) . ?
C44 C45 1.388(10) . ?
C44 H44 0.9500 . ?
C45 C46 1.399(13) . ?
C45 H45 0.9500 . ?
C46 C47 1.380(12) . ?
C46 H46 0.9500 . ?
C47 C48 1.408(9) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C54 1.397(9) . ?
C49 C50 1.410(9) . ?
C50 C51 1.403(9) . ?
C50 H50 0.9500 . ?
C51 C52 1.383(11) . ?
C51 H51 0.9500 . ?
C52 C53 1.391(12) . ?
C52 H52 0.9500 . ?
C53 C54 1.393(10) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.537(7) . ?
C55 C62 1.558(7) . ?
C56 C57 1.520(8) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.525(7) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.529(8) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.516(8) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.520(8) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.530(7) . ?
C62 H62A 0.9900 . ?
C62 H3W 0.9900 . ?
C63 C64 1.521(8) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.506(8) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.517(8) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.518(9) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
Cl1 Cl1A 1.189(13) . ?
Cl1 C70 1.622(14) . ?
Cl1A C70 1.880(15) . ?
Cl2 Cl2A 1.338(12) . ?
Cl2 C70 1.617(15) . ?
Cl2A C70 1.721(14) . ?

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 B1 C19 108.2(4) . . ?
C1 B1 C13 113.0(4) . . ?
C19 B1 C13 118.1(4) . . ?
C1 B1 N1 96.6(4) . . ?
C19 B1 N1 111.0(4) . . ?
C13 B1 N1 107.9(4) . . ?
C31 B2 C49 114.8(4) . . ?
C31 B2 C43 109.5(4) . . ?
C49 B2 C43 116.3(5) . . ?
C31 B2 N2 97.0(4) . . ?
C49 B2 N2 107.1(4) . . ?
C43 B2 N2 110.2(4) . . ?
C11 N1 C7 120.6(5) . . ?
C11 N1 B1 128.1(4) . . ?
C7 N1 B1 111.3(4) . . ?
C41 N2 C37 120.4(4) . . ?
C41 N2 B2 127.7(4) . . ?
C37 N2 B2 111.9(4) . . ?
C2 C1 C6 118.7(4) . . ?
C2 C1 B1 129.7(5) . . ?
C6 C1 B1 111.6(4) . . ?
C1 C2 C3 118.8(5) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C4 121.6(5) . . ?
C2 C3 C33 129.6(5) . . ?
C4 C3 C33 108.6(4) . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 C55 128.0(5) . . ?
C3 C4 C55 111.5(4) . . ?
C4 C5 C6 116.9(5) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
C1 C6 C5 123.4(5) . . ?
C1 C6 C7 109.9(4) . . ?
C5 C6 C7 126.7(5) . . ?
N1 C7 C8 121.0(5) . . ?
N1 C7 C6 110.6(5) . . ?
C8 C7 C6 128.3(5) . . ?
C7 C8 C9 118.6(5) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
C10 C9 C8 119.2(5) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C11 C10 C9 121.2(5) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
N1 C11 C10 119.4(5) . . ?
N1 C11 C12 118.7(5) . . ?
C10 C11 C12 121.9(5) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 116.3(5) . . ?
C18 C13 B1 125.2(5) . . ?
C14 C13 B1 118.4(5) . . ?
C15 C14 C13 121.6(5) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 121.0(6) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C17 118.5(5) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C18 C17 C16 120.1(5) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C13 122.4(5) . . ?
C17 C18 H18 118.8 . . ?
C13 C18 H18 118.8 . . ?
C24 C19 C20 115.5(5) . . ?
C24 C19 B1 119.5(4) . . ?
C20 C19 B1 124.5(5) . . ?
C21 C20 C19 122.2(5) . . ?
C21 C20 H20 118.9 . . ?
C19 C20 H20 118.9 . . ?
C22 C21 C20 120.6(5) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 118.7(5) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C24 C23 C22 120.6(5) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C19 122.5(5) . . ?
C23 C24 H24 118.8 . . ?
C19 C24 H24 118.8 . . ?
C32 C31 C36 116.8(5) . . ?
C32 C31 B2 132.5(5) . . ?
C36 C31 B2 110.6(4) . . ?
C33 C32 C31 120.0(5) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 121.7(5) . . ?
C32 C33 C3 130.1(5) . . ?
C34 C33 C3 108.1(4) . . ?
C35 C34 C33 119.4(5) . . ?
C35 C34 C55 129.7(5) . . ?
C33 C34 C55 110.9(4) . . ?
C34 C35 C36 117.9(5) . . ?
C34 C35 H35 121.1 . . ?
C36 C35 H35 121.1 . . ?
C35 C36 C31 124.1(5) . . ?
C35 C36 C37 125.8(5) . . ?
C31 C36 C37 109.9(4) . . ?
N2 C37 C38 121.8(5) . . ?
N2 C37 C36 110.3(4) . . ?
C38 C37 C36 127.9(5) . . ?
C39 C38 C37 117.5(5) . . ?
C39 C38 H38 121.3 . . ?
C37 C38 H38 121.3 . . ?
C38 C39 C40 120.9(5) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 H39 119.6 . . ?
C39 C40 C41 119.9(5) . . ?
C39 C40 H40 120.1 . . ?
C41 C40 H40 120.1 . . ?
N2 C41 C40 119.5(5) . . ?
N2 C41 C42 119.9(5) . . ?
C40 C41 C42 120.6(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C48 C43 C44 116.4(5) . . ?
C48 C43 B2 124.9(5) . . ?
C44 C43 B2 118.4(5) . . ?
C45 C44 C43 122.0(7) . . ?
C45 C44 H44 119.0 . . ?
C43 C44 H44 119.0 . . ?
C44 C45 C46 120.2(7) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C47 C46 C45 119.0(6) . . ?
C47 C46 H46 120.5 . . ?
C45 C46 H46 120.5 . . ?
C46 C47 C48 120.6(7) . . ?
C46 C47 H47 119.7 . . ?
C48 C47 H47 119.7 . . ?
C43 C48 C47 121.8(6) . . ?
C43 C48 H48 119.1 . . ?
C47 C48 H48 119.1 . . ?
C54 C49 C50 115.7(5) . . ?
C54 C49 B2 125.5(5) . . ?
C50 C49 B2 118.7(5) . . ?
C51 C50 C49 121.9(6) . . ?
C51 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
C52 C51 C50 120.3(7) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C52 C53 119.3(6) . . ?
C51 C52 H52 120.4 . . ?
C53 C52 H52 120.4 . . ?
C52 C53 C54 119.8(7) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C53 C54 C49 123.0(7) . . ?
C53 C54 H54 118.5 . . ?
C49 C54 H54 118.5 . . ?
C4 C55 C34 100.3(4) . . ?
C4 C55 C56 113.6(4) . . ?
C34 C55 C56 113.3(4) . . ?
C4 C55 C62 106.8(4) . . ?
C34 C55 C62 111.0(4) . . ?
C56 C55 C62 111.2(4) . . ?
C57 C56 C55 116.3(4) . . ?
C57 C56 H56A 108.2 . . ?
C55 C56 H56A 108.2 . . ?
C57 C56 H56B 108.2 . . ?
C55 C56 H56B 108.2 . . ?
H56A C56 H56B 107.4 . . ?
C56 C57 C58 113.4(5) . . ?
C56 C57 H57A 108.9 . . ?
C58 C57 H57A 108.9 . . ?
C56 C57 H57B 108.9 . . ?
C58 C57 H57B 108.9 . . ?
H57A C57 H57B 107.7 . . ?
C57 C58 C59 114.1(5) . . ?
C57 C58 H58A 108.7 . . ?
C59 C58 H58A 108.7 . . ?
C57 C58 H58B 108.7 . . ?
C59 C58 H58B 108.7 . . ?
H58A C58 H58B 107.6 . . ?
C60 C59 C58 113.7(5) . . ?
C60 C59 H59A 108.8 . . ?
C58 C59 H59A 108.8 . . ?
C60 C59 H59B 108.8 . . ?
C58 C59 H59B 108.8 . . ?
H59A C59 H59B 107.7 . . ?
C59 C60 C61 114.2(5) . . ?
C59 C60 H60A 108.7 . . ?
C61 C60 H60A 108.7 . . ?
C59 C60 H60B 108.7 . . ?
C61 C60 H60B 108.7 . . ?
H60A C60 H60B 107.6 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C55 117.3(4) . . ?
C63 C62 H62A 108.0 . . ?
C55 C62 H62A 108.0 . . ?
C63 C62 H3W 108.0 . . ?
C55 C62 H3W 108.0 . . ?
H62A C62 H3W 107.2 . . ?
C64 C63 C62 110.6(5) . . ?
C64 C63 H63A 109.5 . . ?
C62 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 108.1 . . ?
C65 C64 C63 116.3(5) . . ?
C65 C64 H64A 108.2 . . ?
C63 C64 H64A 108.2 . . ?
C65 C64 H64B 108.2 . . ?
C63 C64 H64B 108.2 . . ?
H64A C64 H64B 107.4 . . ?
C64 C65 C66 113.1(5) . . ?
C64 C65 H65A 109.0 . . ?
C66 C65 H65A 109.0 . . ?
C64 C65 H65B 109.0 . . ?
C66 C65 H65B 109.0 . . ?
H65A C65 H65B 107.8 . . ?
C65 C66 C67 114.9(5) . . ?
C65 C66 H66A 108.5 . . ?
C67 C66 H66A 108.5 . . ?
C65 C66 H66B 108.5 . . ?
C67 C66 H66B 108.5 . . ?
H66A C66 H66B 107.5 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
Cl1A Cl1 C70 82.4(7) . . ?
Cl1 Cl1A C70 58.8(6) . . ?
Cl2A Cl2 C70 70.5(7) . . ?
Cl2 Cl2A C70 62.4(7) . . ?
Cl2 C70 Cl1 116.1(10) . . ?
Cl2 C70 Cl2A 47.1(5) . . ?
Cl1 C70 Cl2A 123.1(9) . . ?
Cl2 C70 Cl1A 108.2(9) . . ?
Cl1 C70 Cl1A 38.8(5) . . ?
Cl2A C70 Cl1A 89.1(8) . . ?
Cl3 C71 Cl4 112.8(8) . . ?

_refine_diff_density_max         0.858
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.100

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dichloromethane, acetonitrile'
####################################################################### 
# 
# 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_080514RAL_MY_PFPH_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1436392'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;

#======================================================================
# start Validation Reply Form

_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......       0.928      
RESPONSE: Even though we collected data out to 0.81 \%A resolution using
copper radiation, the crystal diffracted poorly between 0.92 and 0.82 \%A
resolution, giving only 81.4% completion in that range.
;
# end Validation Reply Form



_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C61 H42 B2 F20 N2'
_chemical_formula_sum            'C61 H42 B2 F20 N2'
_chemical_formula_weight         1204.58

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   17.8626(6)
_cell_length_b                   9.9345(3)
_cell_length_c                   30.455(1)
_cell_angle_alpha                90
_cell_angle_beta                 102.414(2)
_cell_angle_gamma                90
_cell_volume                     5278.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9875
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      70.22

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_F_000             2448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.175
_exptl_absorpt_coefficient_mu    1.205
_shelx_estimated_absorpt_T_min   0.735
_shelx_estimated_absorpt_T_max   0.817
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_absorpt_special_details   
'crystal mounted on a Cryoloop using Paratone-N'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22253
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.971
_diffrn_reflns_theta_max         70.488
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measured_fraction_theta_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_point_group_measured_fraction_full 0.928
_reflns_number_total             4553
_reflns_number_gt                3738
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          'hexyl groups show disorder'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0724P)²+8.1269P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4553
_refine_ls_number_parameters     414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1445
_refine_ls_wR_factor_gt          0.1372
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.32516(8) -0.13857(15) -0.06773(5) 0.0398(4) Uani 1 1 d . . . . .
F2 F 0.45360(10) -0.23798(18) -0.01715(6) 0.0567(5) Uani 1 1 d . . . . .
F3 F 0.59218(9) -0.1354(2) -0.02212(5) 0.0561(5) Uani 1 1 d . . . . .
F4 F 0.60027(8) 0.06896(19) -0.08041(5) 0.0503(4) Uani 1 1 d . . . . .
F5 F 0.47472(7) 0.16720(16) -0.13243(5) 0.0397(4) Uani 1 1 d . . . . .
F6 F 0.31335(8) -0.20892(15) -0.15592(6) 0.0428(4) Uani 1 1 d . . . . .
F7 F 0.19036(9) -0.35321(16) -0.19107(6) 0.0552(5) Uani 1 1 d . . . . .
F8 F 0.04880(9) -0.23915(17) -0.21090(6) 0.0496(4) Uani 1 1 d . . . . .
F9 F 0.03362(7) 0.02854(17) -0.19374(5) 0.0438(4) Uani 1 1 d . . . . .
F10 F 0.15503(7) 0.17392(14) -0.15667(5) 0.0330(3) Uani 1 1 d . . . . .
N1 N 0.32425(10) 0.2023(2) -0.16325(6) 0.0251(4) Uani 1 1 d . . . . .
C1 C 0.28956(11) 0.1875(2) -0.09043(7) 0.0243(5) Uani 1 1 d . . . . .
C2 C 0.27022(11) 0.1606(2) -0.04942(7) 0.0239(5) Uani 1 1 d . . . . .
H2 H 0.2642 0.0706 -0.0402 0.029 Uiso 1 1 calc R U . . .
C3 C 0.25985(11) 0.2684(2) -0.02223(7) 0.0243(5) Uani 1 1 d . . . . .
C4 C 0.26722(13) 0.4031(2) -0.03512(8) 0.0275(5) Uani 1 1 d . . . . .
C5 C 0.28643(13) 0.4312(2) -0.07581(8) 0.0293(5) Uani 1 1 d . . . . .
H5 H 0.2919 0.5213 -0.0851 0.035 Uiso 1 1 calc R U . . .
C6 C 0.29742(12) 0.3224(2) -0.10272(7) 0.0258(5) Uani 1 1 d . . . . .
C7 C 0.31637(12) 0.3285(2) -0.14712(8) 0.0274(5) Uani 1 1 d . . . . .
C8 C 0.32640(14) 0.4413(3) -0.17195(8) 0.0330(5) Uani 1 1 d . . . . .
H8 H 0.3210 0.5291 -0.1607 0.040 Uiso 1 1 calc R U . . .
C9 C 0.34447(14) 0.4234(3) -0.21341(8) 0.0352(6) Uani 1 1 d . . . . .
H9 H 0.3512 0.4994 -0.2311 0.042 Uiso 1 1 calc R U . . .
C10 C 0.35286(13) 0.2947(3) -0.22924(8) 0.0328(6) Uani 1 1 d . . . . .
H10 H 0.3655 0.2829 -0.2577 0.039 Uiso 1 1 calc R U . . .
C11 C 0.34298(12) 0.1835(3) -0.20390(7) 0.0278(5) Uani 1 1 d . . . . .
C12 C 0.35306(13) 0.0435(3) -0.21926(8) 0.0316(5) Uani 1 1 d . . . . .
H12A H 0.3813 -0.0097 -0.1940 0.047 Uiso 1 1 calc R U . . .
H12B H 0.3819 0.0455 -0.2432 0.047 Uiso 1 1 calc R U . . .
H12C H 0.3027 0.0027 -0.2307 0.047 Uiso 1 1 calc R U . . .
C13 C 0.39303(12) 0.0160(2) -0.10360(7) 0.0259(5) Uani 1 1 d . . . . .
C14 C 0.46522(13) 0.0651(3) -0.10477(8) 0.0301(5) Uani 1 1 d . . . . .
C15 C 0.53194(13) 0.0160(3) -0.07802(8) 0.0353(6) Uani 1 1 d . . . . .
C16 C 0.52845(14) -0.0864(3) -0.04844(9) 0.0395(6) Uani 1 1 d . . . . .
C17 C 0.45774(15) -0.1383(3) -0.04601(9) 0.0388(6) Uani 1 1 d . . . . .
C18 C 0.39264(13) -0.0858(3) -0.07299(8) 0.0314(5) Uani 1 1 d . . . . .
C19 C 0.24031(12) -0.0103(2) -0.15238(7) 0.0251(5) Uani 1 1 d . . . . .
C20 C 0.24484(13) -0.1446(3) -0.16282(9) 0.0332(6) Uani 1 1 d . . . . .
C21 C 0.18189(15) -0.2224(3) -0.18192(9) 0.0379(6) Uani 1 1 d . . . . .
C22 C 0.11011(14) -0.1650(3) -0.19214(8) 0.0368(6) Uani 1 1 d . . . . .
C23 C 0.10277(13) -0.0314(3) -0.18334(8) 0.0321(6) Uani 1 1 d . . . . .
C24 C 0.16724(13) 0.0424(2) -0.16367(7) 0.0279(5) Uani 1 1 d . . . . .
C25 C 0.2500 0.5000(3) 0.0000 0.0313(7) Uani 1 2 d S T P . .
C26 C 0.31967(17) 0.5900(3) 0.01990(9) 0.0447(7) Uani 1 1 d . . . . .
H26A H 0.3259 0.6568 -0.0032 0.054 Uiso 1 1 calc R U . . .
H26B H 0.3079 0.6404 0.0456 0.054 Uiso 1 1 calc R U . . .
C27 C 0.39590(19) 0.5179(4) 0.03583(11) 0.0715(12) Uani 1 1 d . . . . .
H27A H 0.4151 0.4999 0.0088 0.086 Uiso 0.5095 1 d . U P . .
H27B H 0.3837 0.4303 0.0461 0.086 Uiso 0.5095 1 d . U P . .
H27C H 0.4378 0.5770 0.0342 0.086 Uiso 0.4905 1 d . U P . .
H27D H 0.3991 0.4420 0.0160 0.086 Uiso 0.4905 1 d . U P . .
C28 C 0.4611(4) 0.5641(6) 0.06904(18) 0.0523(18) Uani 0.509(5) 1 d . . P . .
H28A H 0.4686 0.6613 0.0643 0.063 Uiso 0.509(5) 1 calc R U P . .
H28B H 0.5075 0.5164 0.0644 0.063 Uiso 0.509(5) 1 calc R U P . .
C28A C 0.4045(3) 0.4670(6) 0.08294(19) 0.0410(15) Uani 0.491(5) 1 d . . P . .
H28C H 0.3769 0.3806 0.0829 0.049 Uiso 0.491(5) 1 calc R U P . .
H28D H 0.3826 0.5327 0.1012 0.049 Uiso 0.491(5) 1 calc R U P . .
C29 C 0.4537(4) 0.5431(7) 0.1159(2) 0.0588(19) Uani 0.509(5) 1 d . . P . .
H29A H 0.4001 0.5621 0.1179 0.071 Uiso 0.509(5) 1 calc R U P . .
H29B H 0.4869 0.6089 0.1354 0.071 Uiso 0.509(5) 1 calc R U P . .
C29A C 0.4911(3) 0.4467(7) 0.10322(19) 0.0416(16) Uani 0.491(5) 1 d . . P . .
H29C H 0.5154 0.5348 0.1124 0.050 Uiso 0.491(5) 1 calc R U P . .
H29D H 0.5163 0.4073 0.0802 0.050 Uiso 0.491(5) 1 calc R U P . .
C30 C 0.4748(6) 0.4015(8) 0.1342(3) 0.061(2) Uani 0.509(5) 1 d . . P . .
H30A H 0.4397 0.3339 0.1169 0.073 Uiso 0.509(5) 1 calc R U P . .
H30B H 0.5280 0.3789 0.1322 0.073 Uiso 0.509(5) 1 calc R U P . .
C30A C 0.5021(3) 0.3516(7) 0.1446(2) 0.0354(15) Uani 0.491(5) 1 d . . P . .
H30C H 0.4788 0.2633 0.1347 0.042 Uiso 0.491(5) 1 calc R U P . .
H30D H 0.5576 0.3371 0.1562 0.042 Uiso 0.491(5) 1 calc R U P . .
C31 C 0.46730(19) 0.4034(4) 0.18264(11) 0.0578(8) Uani 1 1 d . . . . .
H31D H 0.4954 0.4807 0.1980 0.087 Uiso 0.5002 1 calc R U P . .
H31E H 0.4886 0.3201 0.1975 0.087 Uiso 0.5002 1 calc R U P . .
H31F H 0.4131 0.4107 0.1838 0.087 Uiso 0.5002 1 calc R U P . .
H31A H 0.4360 0.3269 0.1882 0.087 Uiso 0.4998 1 calc R U P . .
H31B H 0.4428 0.4876 0.1887 0.087 Uiso 0.4998 1 calc R U P . .
H31C H 0.5183 0.3970 0.2024 0.087 Uiso 0.4998 1 calc R U P . .
B1 B 0.31127(14) 0.0888(3) -0.12782(9) 0.0259(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C18 1.355(3) . ?
F2 C17 1.337(3) . ?
F3 C16 1.335(3) . ?
F4 C15 1.345(3) . ?
F5 C14 1.353(3) . ?
F6 C20 1.356(3) . ?
F7 C21 1.344(3) . ?
F8 C22 1.342(3) . ?
F9 C23 1.346(3) . ?
F10 C24 1.349(3) . ?
N1 C11 1.363(3) . ?
N1 C7 1.364(3) . ?
N1 B1 1.612(3) . ?
C1 C2 1.391(3) . ?
C1 C6 1.407(3) . ?
C1 B1 1.612(3) . ?
C2 C3 1.390(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.409(3) . ?
C3 C3 1.470(4) 2 ?
C4 C5 1.384(3) . ?
C4 C25 1.519(3) . ?
C5 C6 1.396(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.464(3) . ?
C7 C8 1.385(3) . ?
C8 C9 1.380(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.490(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.376(3) . ?
C13 C14 1.386(3) . ?
C13 B1 1.654(3) . ?
C14 C15 1.380(3) . ?
C15 C16 1.369(4) . ?
C16 C17 1.381(4) . ?
C17 C18 1.374(4) . ?
C19 C20 1.378(3) . ?
C19 C24 1.380(3) . ?
C19 B1 1.652(3) . ?
C20 C21 1.386(4) . ?
C21 C22 1.377(4) . ?
C22 C23 1.366(4) . ?
C23 C24 1.388(3) . ?
C25 C4 1.519(3) 2 ?
C25 C26 1.546(3) . ?
C25 C26 1.546(3) 2 ?
C26 C27 1.523(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.444(6) . ?
C27 C28A 1.498(6) . ?
C27 H27A 0.9739 . ?
C27 H27B 0.9653 . ?
C27 H27C 0.9610 . ?
C27 H27D 0.9753 . ?
C28 C29 1.477(8) . ?
C28 H27C 1.0611 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28A C29A 1.551(7) . ?
C28A H27B 1.1622 . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C29 C30 1.530(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29A C30A 1.553(9) . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C30 C31 1.510(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30A C31 1.518(7) . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C31 H31D 0.9800 . ?
C31 H31E 0.9800 . ?
C31 H31F 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 N1 C7 121.2(2) . . ?
C11 N1 B1 127.6(2) . . ?
C7 N1 B1 111.16(18) . . ?
C2 C1 C6 118.7(2) . . ?
C2 C1 B1 131.4(2) . . ?
C6 C1 B1 109.81(19) . . ?
C3 C2 C1 118.5(2) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 122.2(2) . . ?
C2 C3 C3 129.60(13) . 2 ?
C4 C3 C3 108.17(13) . 2 ?
C5 C4 C3 119.9(2) . . ?
C5 C4 C25 129.0(2) . . ?
C3 C4 C25 111.2(2) . . ?
C4 C5 C6 117.5(2) . . ?
C4 C5 H5 121.2 . . ?
C6 C5 H5 121.2 . . ?
C5 C6 C1 123.2(2) . . ?
C5 C6 C7 126.9(2) . . ?
C1 C6 C7 109.9(2) . . ?
N1 C7 C8 120.8(2) . . ?
N1 C7 C6 110.9(2) . . ?
C8 C7 C6 128.3(2) . . ?
C9 C8 C7 118.6(2) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C8 C9 C10 120.1(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 120.5(2) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
N1 C11 C10 118.9(2) . . ?
N1 C11 C12 118.9(2) . . ?
C10 C11 C12 122.2(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 114.6(2) . . ?
C18 C13 B1 119.38(19) . . ?
C14 C13 B1 124.9(2) . . ?
F5 C14 C15 115.1(2) . . ?
F5 C14 C13 121.5(2) . . ?
C15 C14 C13 123.4(2) . . ?
F4 C15 C16 119.8(2) . . ?
F4 C15 C14 120.5(2) . . ?
C16 C15 C14 119.7(2) . . ?
F3 C16 C15 120.8(2) . . ?
F3 C16 C17 120.2(3) . . ?
C15 C16 C17 119.0(2) . . ?
F2 C17 C18 121.0(2) . . ?
F2 C17 C16 119.5(2) . . ?
C18 C17 C16 119.5(2) . . ?
F1 C18 C17 116.3(2) . . ?
F1 C18 C13 119.9(2) . . ?
C17 C18 C13 123.8(2) . . ?
C20 C19 C24 114.2(2) . . ?
C20 C19 B1 127.2(2) . . ?
C24 C19 B1 118.7(2) . . ?
F6 C20 C19 121.1(2) . . ?
F6 C20 C21 115.2(2) . . ?
C19 C20 C21 123.7(2) . . ?
F7 C21 C22 119.7(2) . . ?
F7 C21 C20 120.6(2) . . ?
C22 C21 C20 119.7(2) . . ?
F8 C22 C23 120.9(2) . . ?
F8 C22 C21 120.3(2) . . ?
C23 C22 C21 118.9(2) . . ?
F9 C23 C22 120.4(2) . . ?
F9 C23 C24 120.1(2) . . ?
C22 C23 C24 119.5(2) . . ?
F10 C24 C19 120.3(2) . . ?
F10 C24 C23 115.6(2) . . ?
C19 C24 C23 124.1(2) . . ?
C4 C25 C4 101.3(3) . 2 ?
C4 C25 C26 112.01(14) . . ?
C4 C25 C26 111.00(13) 2 . ?
C4 C25 C26 111.00(13) . 2 ?
C4 C25 C26 112.01(14) 2 2 ?
C26 C25 C26 109.4(3) . 2 ?
C27 C26 C25 116.3(3) . . ?
C27 C26 H26A 108.2 . . ?
C25 C26 H26A 108.2 . . ?
C27 C26 H26B 108.2 . . ?
C25 C26 H26B 108.2 . . ?
H26A C26 H26B 107.4 . . ?
C28 C27 C28A 62.3(3) . . ?
C28 C27 C26 127.3(5) . . ?
C28A C27 C26 111.4(3) . . ?
C28 C27 H27A 105.8 . . ?
C28A C27 H27A 139.9 . . ?
C26 C27 H27A 105.7 . . ?
C28 C27 H27B 105.3 . . ?
C28A C27 H27B 50.9 . . ?
C26 C27 H27B 106.2 . . ?
H27A C27 H27B 104.7 . . ?
C28 C27 H27C 47.3 . . ?
C28A C27 H27C 109.6 . . ?
C26 C27 H27C 110.4 . . ?
H27A C27 H27C 69.4 . . ?
H27B C27 H27C 143.1 . . ?
C28 C27 H27D 122.3 . . ?
C28A C27 H27D 108.9 . . ?
C26 C27 H27D 109.5 . . ?
H27A C27 H27D 42.0 . . ?
H27B C27 H27D 63.3 . . ?
H27C C27 H27D 106.9 . . ?
C27 C28 C29 113.9(5) . . ?
C27 C28 H27C 41.7 . . ?
C29 C28 H27C 152.4 . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28A 108.8 . . ?
H27C C28 H28A 76.8 . . ?
C27 C28 H28B 108.8 . . ?
C29 C28 H28B 108.8 . . ?
H27C C28 H28B 94.4 . . ?
H28A C28 H28B 107.7 . . ?
C27 C28A C29A 108.3(4) . . ?
C27 C28A H27B 40.1 . . ?
C29A C28A H27B 115.4 . . ?
C27 C28A H28C 110.0 . . ?
C29A C28A H28C 110.0 . . ?
H27B C28A H28C 70.8 . . ?
C27 C28A H28D 110.0 . . ?
C29A C28A H28D 110.0 . . ?
H27B C28A H28D 131.7 . . ?
H28C C28A H28D 108.4 . . ?
C28 C29 C30 114.5(7) . . ?
C28 C29 H29A 108.6 . . ?
C30 C29 H29A 108.6 . . ?
C28 C29 H29B 108.6 . . ?
C30 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C28A C29A C30A 110.0(5) . . ?
C28A C29A H29C 109.7 . . ?
C30A C29A H29C 109.7 . . ?
C28A C29A H29D 109.7 . . ?
C30A C29A H29D 109.7 . . ?
H29C C29A H29D 108.2 . . ?
C31 C30 C29 106.0(7) . . ?
C31 C30 H30A 110.5 . . ?
C29 C30 H30A 110.5 . . ?
C31 C30 H30B 110.5 . . ?
C29 C30 H30B 110.5 . . ?
H30A C30 H30B 108.7 . . ?
C31 C30A C29A 114.4(5) . . ?
C31 C30A H30C 108.7 . . ?
C29A C30A H30C 108.7 . . ?
C31 C30A H30D 108.7 . . ?
C29A C30A H30D 108.7 . . ?
H30C C30A H30D 107.6 . . ?
C30 C31 C30A 27.4(3) . . ?
C30 C31 H31D 109.5 . . ?
C30A C31 H31D 112.3 . . ?
C30 C31 H31E 109.5 . . ?
C30A C31 H31E 83.4 . . ?
H31D C31 H31E 109.5 . . ?
C30 C31 H31F 109.5 . . ?
C30A C31 H31F 128.5 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30A C31 H31A 102.2 . . ?
H31D C31 H31A 141.1 . . ?
H31E C31 H31A 56.3 . . ?
H31F C31 H31A 56.3 . . ?
C30 C31 H31B 109.5 . . ?
C30A C31 H31B 135.0 . . ?
H31D C31 H31B 56.3 . . ?
H31E C31 H31B 141.1 . . ?
H31F C31 H31B 56.3 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C30A C31 H31C 88.2 . . ?
H31D C31 H31C 56.3 . . ?
H31E C31 H31C 56.3 . . ?
H31F C31 H31C 141.1 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 B1 N1 97.94(18) . . ?
C1 B1 C19 113.87(17) . . ?
N1 B1 C19 108.71(17) . . ?
C1 B1 C13 105.93(18) . . ?
N1 B1 C13 111.36(17) . . ?
C19 B1 C13 117.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.3(3) . . . . ?
B1 C1 C2 C3 175.1(2) . . . . ?
C1 C2 C3 C4 0.9(3) . . . . ?
C1 C2 C3 C3 -179.5(3) . . . 2 ?
C2 C3 C4 C5 -0.9(3) . . . . ?
C3 C3 C4 C5 179.4(2) 2 . . . ?
C2 C3 C4 C25 177.86(17) . . . . ?
C3 C3 C4 C25 -1.8(3) 2 . . . ?
C3 C4 C5 C6 0.3(3) . . . . ?
C25 C4 C5 C6 -178.24(18) . . . . ?
C4 C5 C6 C1 0.3(3) . . . . ?
C4 C5 C6 C7 178.7(2) . . . . ?
C2 C1 C6 C5 -0.3(3) . . . . ?
B1 C1 C6 C5 -176.6(2) . . . . ?
C2 C1 C6 C7 -178.93(18) . . . . ?
B1 C1 C6 C7 4.8(2) . . . . ?
C11 N1 C7 C8 0.7(3) . . . . ?
B1 N1 C7 C8 179.0(2) . . . . ?
C11 N1 C7 C6 -179.05(18) . . . . ?
B1 N1 C7 C6 -0.8(2) . . . . ?
C5 C6 C7 N1 178.9(2) . . . . ?
C1 C6 C7 N1 -2.5(3) . . . . ?
C5 C6 C7 C8 -0.9(4) . . . . ?
C1 C6 C7 C8 177.7(2) . . . . ?
N1 C7 C8 C9 0.1(3) . . . . ?
C6 C7 C8 C9 179.8(2) . . . . ?
C7 C8 C9 C10 -0.5(4) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C7 N1 C11 C10 -1.0(3) . . . . ?
B1 N1 C11 C10 -178.96(19) . . . . ?
C7 N1 C11 C12 178.24(19) . . . . ?
B1 N1 C11 C12 0.3(3) . . . . ?
C9 C10 C11 N1 0.5(3) . . . . ?
C9 C10 C11 C12 -178.7(2) . . . . ?
C18 C13 C14 F5 -178.5(2) . . . . ?
B1 C13 C14 F5 -11.0(4) . . . . ?
C18 C13 C14 C15 0.7(4) . . . . ?
B1 C13 C14 C15 168.2(2) . . . . ?
F5 C14 C15 F4 0.0(4) . . . . ?
C13 C14 C15 F4 -179.3(2) . . . . ?
F5 C14 C15 C16 179.2(2) . . . . ?
C13 C14 C15 C16 -0.1(4) . . . . ?
F4 C15 C16 F3 -0.6(4) . . . . ?
C14 C15 C16 F3 -179.8(2) . . . . ?
F4 C15 C16 C17 179.1(2) . . . . ?
C14 C15 C16 C17 -0.1(4) . . . . ?
F3 C16 C17 F2 -0.1(4) . . . . ?
C15 C16 C17 F2 -179.8(2) . . . . ?
F3 C16 C17 C18 179.3(2) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
F2 C17 C18 F1 1.5(4) . . . . ?
C16 C17 C18 F1 -177.9(2) . . . . ?
F2 C17 C18 C13 -179.5(2) . . . . ?
C16 C17 C18 C13 1.1(4) . . . . ?
C14 C13 C18 F1 177.7(2) . . . . ?
B1 C13 C18 F1 9.4(3) . . . . ?
C14 C13 C18 C17 -1.2(4) . . . . ?
B1 C13 C18 C17 -169.5(2) . . . . ?
C24 C19 C20 F6 176.5(2) . . . . ?
B1 C19 C20 F6 -4.5(4) . . . . ?
C24 C19 C20 C21 -1.6(4) . . . . ?
B1 C19 C20 C21 177.4(2) . . . . ?
F6 C20 C21 F7 2.1(4) . . . . ?
C19 C20 C21 F7 -179.7(2) . . . . ?
F6 C20 C21 C22 -177.1(2) . . . . ?
C19 C20 C21 C22 1.1(4) . . . . ?
F7 C21 C22 F8 0.4(4) . . . . ?
C20 C21 C22 F8 179.6(2) . . . . ?
F7 C21 C22 C23 -178.9(2) . . . . ?
C20 C21 C22 C23 0.4(4) . . . . ?
F8 C22 C23 F9 -0.6(4) . . . . ?
C21 C22 C23 F9 178.7(2) . . . . ?
F8 C22 C23 C24 179.6(2) . . . . ?
C21 C22 C23 C24 -1.2(4) . . . . ?
C20 C19 C24 F10 -177.8(2) . . . . ?
B1 C19 C24 F10 3.2(3) . . . . ?
C20 C19 C24 C23 0.8(3) . . . . ?
B1 C19 C24 C23 -178.3(2) . . . . ?
F9 C23 C24 F10 -0.6(3) . . . . ?
C22 C23 C24 F10 179.2(2) . . . . ?
F9 C23 C24 C19 -179.2(2) . . . . ?
C22 C23 C24 C19 0.6(4) . . . . ?
C5 C4 C25 C4 179.4(3) . . . 2 ?
C3 C4 C25 C4 0.72(11) . . . 2 ?
C5 C4 C25 C26 -62.3(3) . . . . ?
C3 C4 C25 C26 119.1(2) . . . . ?
C5 C4 C25 C26 60.3(3) . . . 2 ?
C3 C4 C25 C26 -118.3(2) . . . 2 ?
C4 C25 C26 C27 -49.3(3) . . . . ?
C4 C25 C26 C27 63.1(3) 2 . . . ?
C26 C25 C26 C27 -172.8(3) 2 . . . ?
C25 C26 C27 C28 -155.8(4) . . . . ?
C25 C26 C27 C28A -85.0(4) . . . . ?
C28A C27 C28 C29 -17.2(5) . . . . ?
C26 C27 C28 C29 79.6(6) . . . . ?
C28 C27 C28A C29A -36.3(5) . . . . ?
C26 C27 C28A C29A -158.2(4) . . . . ?
C27 C28 C29 C30 82.6(8) . . . . ?
C27 C28A C29A C30A -161.2(5) . . . . ?
C28 C29 C30 C31 177.2(5) . . . . ?
C28A C29A C30A C31 -60.7(6) . . . . ?
C29 C30 C31 C30A -151.5(13) . . . . ?
C29A C30A C31 C30 19.2(7) . . . . ?
C2 C1 B1 N1 179.6(2) . . . . ?
C6 C1 B1 N1 -4.7(2) . . . . ?
C2 C1 B1 C19 65.0(3) . . . . ?
C6 C1 B1 C19 -119.3(2) . . . . ?
C2 C1 B1 C13 -65.4(3) . . . . ?
C6 C1 B1 C13 110.2(2) . . . . ?
C11 N1 B1 C1 -178.63(18) . . . . ?
C7 N1 B1 C1 3.3(2) . . . . ?
C11 N1 B1 C19 -60.0(3) . . . . ?
C7 N1 B1 C19 121.86(19) . . . . ?
C11 N1 B1 C13 70.8(3) . . . . ?
C7 N1 B1 C13 -107.3(2) . . . . ?
C20 C19 B1 C1 -138.1(2) . . . . ?
C24 C19 B1 C1 40.8(3) . . . . ?
C20 C19 B1 N1 113.9(3) . . . . ?
C24 C19 B1 N1 -67.2(2) . . . . ?
C20 C19 B1 C13 -13.6(3) . . . . ?
C24 C19 B1 C13 165.3(2) . . . . ?
C18 C13 B1 C1 76.0(3) . . . . ?
C14 C13 B1 C1 -91.0(3) . . . . ?
C18 C13 B1 N1 -178.6(2) . . . . ?
C14 C13 B1 N1 14.4(3) . . . . ?
C18 C13 B1 C19 -52.4(3) . . . . ?
C14 C13 B1 C19 140.6(2) . . . . ?

_refine_diff_density_max         0.476
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.054



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: diethyl ether, acetonitrile'
