# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2017

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1521490'
_audit_update_record             
;
2016-12-08 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H48 B2'
_chemical_formula_weight         622.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   6.9356(5)
_cell_length_b                   11.2669(9)
_cell_length_c                   12.5929(13)
_cell_angle_alpha                69.417(8)
_cell_angle_beta                 88.074(7)
_cell_angle_gamma                78.462(6)
_cell_volume                     901.89(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3492
_cell_measurement_theta_min      3.7020
_cell_measurement_theta_max      28.8890

_exptl_crystal_description       'transparent prism'
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_F_000             334
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.089
_exptl_absorpt_coefficient_mu    0.063
_shelx_estimated_absorpt_T_min   0.989
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3385
_diffrn_reflns_number            8238
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.000
_diffrn_reflns_theta_max         29.237
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4241
_reflns_number_gt                3342
_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       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Giacovazzo et al., 1994)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+0.3130P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4241
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1307
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
C1 C 0.1433(2) 0.29975(14) 0.55455(13) 0.0290(3) Uani 1 1 d . . . . .
H1 H 0.0597 0.3671 0.5728 0.035 Uiso 1 1 calc R U . . .
C2 C 0.2478(2) 0.21568(13) 0.53172(11) 0.0220(3) Uani 1 1 d . . . . .
C3 C 0.3760(2) 0.10870(13) 0.51175(11) 0.0204(3) Uani 1 1 d . . . . .
C4 C 0.4376(2) 0.11468(13) 0.40215(11) 0.0205(3) Uani 1 1 d . . . . .
C5 C 0.5603(2) 0.00383(13) 0.39426(11) 0.0208(3) Uani 1 1 d . . . . .
H5 H 0.6026 0.0048 0.3215 0.025 Uiso 1 1 calc R U . . .
C6 C 0.3564(2) 0.37852(12) 0.28739(11) 0.0201(3) Uani 1 1 d . . . . .
C7 C 0.4973(2) 0.41488(13) 0.34166(11) 0.0229(3) Uani 1 1 d . . . . .
C8 C 0.4726(2) 0.54195(14) 0.33918(12) 0.0264(3) Uani 1 1 d . . . . .
H8 H 0.5700 0.5647 0.3754 0.032 Uiso 1 1 calc R U . . .
C9 C 0.3103(2) 0.63550(13) 0.28543(12) 0.0261(3) Uani 1 1 d . . . . .
C10 C 0.1724(2) 0.60015(13) 0.23160(12) 0.0257(3) Uani 1 1 d . . . . .
H10 H 0.0599 0.6634 0.1946 0.031 Uiso 1 1 calc R U . . .
C11 C 0.1923(2) 0.47550(13) 0.22969(11) 0.0221(3) Uani 1 1 d . . . . .
C12 C 0.6818(2) 0.32164(15) 0.40103(14) 0.0326(4) Uani 1 1 d . . . . .
H12A H 0.7830 0.3701 0.4038 0.049 Uiso 1 1 calc R U . . .
H12B H 0.7297 0.2633 0.3594 0.049 Uiso 1 1 calc R U . . .
H12C H 0.6525 0.2709 0.4785 0.049 Uiso 1 1 calc R U . . .
C13 C 0.2847(3) 0.77234(15) 0.28338(15) 0.0363(4) Uani 1 1 d . . . . .
H13A H 0.2694 0.8324 0.2046 0.055 Uiso 1 1 calc R U . . .
H13B H 0.4007 0.7814 0.3199 0.055 Uiso 1 1 calc R U . . .
H13C H 0.1672 0.7922 0.3244 0.055 Uiso 1 1 calc R U . . .
C14 C 0.0346(2) 0.45017(15) 0.16612(14) 0.0329(4) Uani 1 1 d . . . . .
H14A H -0.0729 0.5264 0.1417 0.049 Uiso 1 1 calc R U . . .
H14B H -0.0163 0.3753 0.2158 0.049 Uiso 1 1 calc R U . . .
H14C H 0.0901 0.4323 0.0994 0.049 Uiso 1 1 calc R U . . .
C15 C 0.3509(2) 0.20622(12) 0.17859(11) 0.0204(3) Uani 1 1 d . . . . .
C16 C 0.4649(2) 0.25101(13) 0.08290(11) 0.0227(3) Uani 1 1 d . . . . .
C17 C 0.4361(2) 0.22328(14) -0.01411(12) 0.0264(3) Uani 1 1 d . . . . .
H17 H 0.5146 0.2532 -0.0775 0.032 Uiso 1 1 calc R U . . .
C18 C 0.2968(2) 0.15339(14) -0.02123(12) 0.0267(3) Uani 1 1 d . . . . .
C19 C 0.1828(2) 0.11152(14) 0.07237(12) 0.0258(3) Uani 1 1 d . . . . .
H19 H 0.0841 0.0655 0.0684 0.031 Uiso 1 1 calc R U . . .
C20 C 0.2092(2) 0.13504(13) 0.17177(12) 0.0231(3) Uani 1 1 d . . . . .
C21 C 0.6240(2) 0.32490(16) 0.08423(13) 0.0319(4) Uani 1 1 d . . . . .
H21A H 0.6818 0.3510 0.0095 0.048 Uiso 1 1 calc R U . . .
H21B H 0.7266 0.2695 0.1418 0.048 Uiso 1 1 calc R U . . .
H21C H 0.5667 0.4021 0.1023 0.048 Uiso 1 1 calc R U . . .
C22 C 0.2744(3) 0.12032(17) -0.12587(13) 0.0355(4) Uani 1 1 d . . . . .
H22A H 0.2859 0.1949 -0.1938 0.053 Uiso 1 1 calc R U . . .
H22B H 0.1450 0.0985 -0.1277 0.053 Uiso 1 1 calc R U . . .
H22C H 0.3777 0.0461 -0.1240 0.053 Uiso 1 1 calc R U . . .
C23 C 0.0791(2) 0.08584(15) 0.26990(13) 0.0298(3) Uani 1 1 d . . . . .
H23A H -0.0310 0.0594 0.2434 0.045 Uiso 1 1 calc R U . . .
H23B H 0.0279 0.1548 0.3000 0.045 Uiso 1 1 calc R U . . .
H23C H 0.1562 0.0115 0.3298 0.045 Uiso 1 1 calc R U . . .
B1 B 0.3793(2) 0.23616(15) 0.28945(13) 0.0204(3) 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
C1 C2 1.186(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.4409(19) . ?
C3 C5 1.4000(18) 2_656 ?
C3 C4 1.4136(19) . ?
C4 C5 1.3964(18) . ?
C4 B1 1.5819(19) . ?
C5 C3 1.3999(18) 2_656 ?
C5 H5 0.9500 . ?
C6 C7 1.411(2) . ?
C6 C11 1.4205(19) . ?
C6 B1 1.571(2) . ?
C7 C8 1.397(2) . ?
C7 C12 1.508(2) . ?
C8 C9 1.382(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(2) . ?
C9 C13 1.507(2) . ?
C10 C11 1.3921(19) . ?
C10 H10 0.9500 . ?
C11 C14 1.504(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.409(2) . ?
C15 C16 1.4139(19) . ?
C15 B1 1.574(2) . ?
C16 C17 1.393(2) . ?
C16 C21 1.513(2) . ?
C17 C18 1.386(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.390(2) . ?
C18 C22 1.511(2) . ?
C19 C20 1.392(2) . ?
C19 H19 0.9500 . ?
C20 C23 1.514(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 180.0 . . ?
C1 C2 C3 176.28(15) . . ?
C5 C3 C4 120.10(12) 2_656 . ?
C5 C3 C2 117.58(12) 2_656 . ?
C4 C3 C2 122.31(12) . . ?
C5 C4 C3 116.60(12) . . ?
C5 C4 B1 118.15(12) . . ?
C3 C4 B1 125.24(12) . . ?
C4 C5 C3 123.29(12) . 2_656 ?
C4 C5 H5 118.4 . . ?
C3 C5 H5 118.4 2_656 . ?
C7 C6 C11 117.74(12) . . ?
C7 C6 B1 121.61(12) . . ?
C11 C6 B1 120.64(13) . . ?
C8 C7 C6 120.43(13) . . ?
C8 C7 C12 117.17(14) . . ?
C6 C7 C12 122.38(13) . . ?
C9 C8 C7 121.80(14) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 117.84(13) . . ?
C8 C9 C13 121.44(15) . . ?
C10 C9 C13 120.71(14) . . ?
C9 C10 C11 122.55(13) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 H10 118.7 . . ?
C10 C11 C6 119.60(14) . . ?
C10 C11 C14 117.40(13) . . ?
C6 C11 C14 123.00(12) . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 118.21(13) . . ?
C20 C15 B1 120.69(12) . . ?
C16 C15 B1 121.10(13) . . ?
C17 C16 C15 119.81(14) . . ?
C17 C16 C21 118.56(13) . . ?
C15 C16 C21 121.59(13) . . ?
C18 C17 C16 122.18(14) . . ?
C18 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
C17 C18 C19 117.78(13) . . ?
C17 C18 C22 121.00(14) . . ?
C19 C18 C22 121.20(15) . . ?
C18 C19 C20 121.90(14) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 . . ?
C19 C20 C15 120.10(13) . . ?
C19 C20 C23 118.55(14) . . ?
C15 C20 C23 121.32(13) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C6 B1 C15 121.79(11) . . ?
C6 B1 C4 122.04(12) . . ?
C15 B1 C4 116.15(12) . . ?

_refine_diff_density_max         0.247
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.044

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1521412'
_audit_update_record             
;
2016-12-08 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60.50 H63 B2 Cl N6'
_chemical_formula_weight         931.24

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   13.9954(7)
_cell_length_b                   14.3264(6)
_cell_length_c                   14.4940(7)
_cell_angle_alpha                69.831(4)
_cell_angle_beta                 78.920(4)
_cell_angle_gamma                85.791(4)
_cell_volume                     2677.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7460
_cell_measurement_theta_min      3.1920
_cell_measurement_theta_max      73.3420

_exptl_crystal_description       'transparent prism'
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_F_000             990
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.105
_exptl_absorpt_coefficient_mu    0.959
_shelx_estimated_absorpt_T_min   0.779
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3385
_diffrn_reflns_number            19208
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.218
_diffrn_reflns_theta_max         74.112
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10567
_reflns_number_gt                8399
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0643P)²+2.7338P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10567
_refine_ls_number_parameters     654
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1969
_refine_ls_wR_factor_gt          0.1873
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_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
C1 C 0.99983(18) 0.01891(17) 0.39617(18) 0.0312(5) Uani 1 1 d . . . . .
C2 C 0.96900(18) 0.08929(17) 0.44388(18) 0.0315(5) Uani 1 1 d . . . . .
C3 C 0.96732(18) 0.07228(18) 0.54483(18) 0.0325(5) Uani 1 1 d . . . . .
H3 H 0.9441 0.1222 0.5731 0.039 Uiso 1 1 calc R U . . .
C4 C 0.94245(19) 0.18134(18) 0.37044(18) 0.0336(5) Uani 1 1 d . . . . .
C5 C 0.9034(2) 0.27360(18) 0.36142(19) 0.0377(6) Uani 1 1 d . . . . .
H5 H 0.8807 0.3005 0.4132 0.045 Uiso 1 1 calc R U . . .
C6 C 0.8718(2) 0.41812(18) 0.21323(19) 0.0375(6) Uani 1 1 d . . . . .
C7 C 0.9241(2) 0.4773(2) 0.1244(2) 0.0536(8) Uani 1 1 d . . . . .
H7 H 0.9808 0.4524 0.0925 0.064 Uiso 1 1 calc R U . . .
C8 C 0.8923(3) 0.5745(2) 0.0820(2) 0.0608(9) Uani 1 1 d . . . . .
H8 H 0.9286 0.6161 0.0210 0.073 Uiso 1 1 calc R U . . .
C9 C 0.8101(2) 0.6118(2) 0.1260(2) 0.0516(7) Uani 1 1 d . . . . .
C10 C 0.7591(2) 0.5503(2) 0.2153(2) 0.0514(7) Uani 1 1 d . . . . .
H10 H 0.7019 0.5748 0.2469 0.062 Uiso 1 1 calc R U . . .
C11 C 0.7896(2) 0.4541(2) 0.2594(2) 0.0445(6) Uani 1 1 d . . . . .
H11 H 0.7542 0.4131 0.3211 0.053 Uiso 1 1 calc R U . . .
C12 C 0.7761(3) 0.7177(2) 0.0807(3) 0.0720(11) Uani 1 1 d . . . . .
H12A H 0.8050 0.7610 0.1075 0.108 Uiso 1 1 calc R U . . .
H12B H 0.7050 0.7211 0.0973 0.108 Uiso 1 1 calc R U . . .
H12C H 0.7965 0.7398 0.0080 0.108 Uiso 1 1 calc R U . . .
C13 C 1.11219(19) 0.05053(19) 0.22413(18) 0.0341(5) Uani 1 1 d . . . . .
C14 C 1.1404(2) -0.0413(2) 0.21026(19) 0.0382(6) Uani 1 1 d . . . . .
C15 C 1.2386(2) -0.0623(2) 0.1822(2) 0.0499(7) Uani 1 1 d . . . . .
H15 H 1.2556 -0.1245 0.1732 0.060 Uiso 1 1 calc R U . . .
C16 C 1.3121(2) 0.0042(3) 0.1669(2) 0.0545(8) Uani 1 1 d . . . . .
C17 C 1.2846(2) 0.0939(3) 0.1775(2) 0.0510(7) Uani 1 1 d . . . . .
H17 H 1.3335 0.1415 0.1653 0.061 Uiso 1 1 calc R U . . .
C18 C 1.1876(2) 0.1185(2) 0.2055(2) 0.0432(6) Uani 1 1 d . . . . .
C19 C 1.0687(2) -0.1213(2) 0.2242(2) 0.0428(6) Uani 1 1 d . . . . .
H19A H 1.0336 -0.1010 0.1680 0.064 Uiso 1 1 calc R U . . .
H19B H 1.0221 -0.1310 0.2866 0.064 Uiso 1 1 calc R U . . .
H19C H 1.1039 -0.1837 0.2272 0.064 Uiso 1 1 calc R U . . .
C20 C 1.4180(3) -0.0224(4) 0.1411(3) 0.0789(12) Uani 1 1 d . . . . .
H20A H 1.4448 0.0197 0.0730 0.118 Uiso 1 1 calc R U . . .
H20B H 1.4235 -0.0924 0.1457 0.118 Uiso 1 1 calc R U . . .
H20C H 1.4544 -0.0118 0.1880 0.118 Uiso 1 1 calc R U . . .
C21 C 1.1692(3) 0.2208(3) 0.2138(3) 0.0593(8) Uani 1 1 d . . . . .
H21A H 1.2305 0.2574 0.1925 0.089 Uiso 1 1 calc R U . . .
H21B H 1.1424 0.2145 0.2833 0.089 Uiso 1 1 calc R U . . .
H21C H 1.1227 0.2569 0.1710 0.089 Uiso 1 1 calc R U . . .
C22 C 0.91490(17) 0.03318(17) 0.22696(17) 0.0292(5) Uani 1 1 d . . . . .
C23 C 0.83283(18) -0.02536(18) 0.28314(18) 0.0338(5) Uani 1 1 d . . . . .
C24 C 0.76594(19) -0.04971(19) 0.2354(2) 0.0369(5) Uani 1 1 d . . . . .
H24 H 0.7128 -0.0912 0.2751 0.044 Uiso 1 1 calc R U . . .
C25 C 0.77368(19) -0.01600(19) 0.1328(2) 0.0373(6) Uani 1 1 d . . . . .
C26 C 0.85295(19) 0.04324(18) 0.07722(19) 0.0355(5) Uani 1 1 d . . . . .
H26 H 0.8601 0.0676 0.0065 0.043 Uiso 1 1 calc R U . . .
C27 C 0.92217(18) 0.06812(17) 0.12136(18) 0.0327(5) Uani 1 1 d . . . . .
C28 C 0.8112(2) -0.0647(2) 0.39624(19) 0.0421(6) Uani 1 1 d . . . . .
H28A H 0.7458 -0.0933 0.4191 0.063 Uiso 1 1 calc R U . . .
H28B H 0.8146 -0.0102 0.4217 0.063 Uiso 1 1 calc R U . . .
H28C H 0.8592 -0.1161 0.4211 0.063 Uiso 1 1 calc R U . . .
C29 C 0.6967(2) -0.0382(2) 0.0833(2) 0.0499(7) Uani 1 1 d . . . . .
H29A H 0.6518 -0.0879 0.1330 0.075 Uiso 1 1 calc R U . . .
H29B H 0.7278 -0.0639 0.0302 0.075 Uiso 1 1 calc R U . . .
H29C H 0.6606 0.0230 0.0545 0.075 Uiso 1 1 calc R U . . .
C30 C 1.00474(19) 0.13346(19) 0.05142(18) 0.0368(5) Uani 1 1 d . . . . .
H30A H 1.0636 0.0928 0.0460 0.055 Uiso 1 1 calc R U . . .
H30B H 1.0170 0.1851 0.0778 0.055 Uiso 1 1 calc R U . . .
H30C H 0.9870 0.1648 -0.0147 0.055 Uiso 1 1 calc R U . . .
C40 C 0.51105(18) 0.10137(18) 0.49295(19) 0.0346(5) Uani 1 1 d . . . . .
C41 C 0.54590(19) 0.06499(18) 0.41372(19) 0.0345(5) Uani 1 1 d . . . . .
C42 C 0.53642(19) -0.03313(18) 0.41905(19) 0.0351(5) Uani 1 1 d . . . . .
H42 H 0.5622 -0.0531 0.3631 0.042 Uiso 1 1 calc R U . . .
C43 C 0.5897(2) 0.14702(18) 0.32694(19) 0.0357(5) Uani 1 1 d . . . . .
C44 C 0.6412(2) 0.16878(19) 0.2319(2) 0.0404(6) Uani 1 1 d . . . . .
H44 H 0.6630 0.1239 0.1969 0.048 Uiso 1 1 calc R U . . .
C45 C 0.7021(2) 0.33088(19) 0.10170(19) 0.0409(6) Uani 1 1 d . . . . .
C46 C 0.6693(3) 0.4278(2) 0.0621(2) 0.0599(9) Uani 1 1 d . . . . .
H46 H 0.6170 0.4541 0.0984 0.072 Uiso 1 1 calc R U . . .
C47 C 0.7152(3) 0.4850(2) -0.0318(3) 0.0652(10) Uani 1 1 d . . . . .
H47 H 0.6943 0.5518 -0.0599 0.078 Uiso 1 1 calc R U . . .
C48 C 0.7918(3) 0.4469(2) -0.0867(2) 0.0520(8) Uani 1 1 d . . . . .
C49 C 0.8205(3) 0.3504(2) -0.0439(2) 0.0549(8) Uani 1 1 d . . . . .
H49 H 0.8720 0.3230 -0.0800 0.066 Uiso 1 1 calc R U . . .
C50 C 0.7761(2) 0.2914(2) 0.0512(2) 0.0507(7) Uani 1 1 d . . . . .
H50 H 0.7974 0.2249 0.0800 0.061 Uiso 1 1 calc R U . . .
C51 C 0.8399(3) 0.5097(3) -0.1908(2) 0.0683(10) Uani 1 1 d . . . . .
H51A H 0.8967 0.4741 -0.2138 0.103 Uiso 1 1 calc R U . . .
H51B H 0.8606 0.5729 -0.1893 0.103 Uiso 1 1 calc R U . . .
H51C H 0.7934 0.5226 -0.2365 0.103 Uiso 1 1 calc R U . . .
C52 C 0.61182(18) 0.26583(18) 0.49797(18) 0.0329(5) Uani 1 1 d . . . . .
C53 C 0.68210(19) 0.20655(19) 0.55160(19) 0.0361(5) Uani 1 1 d . . . . .
C54 C 0.7460(2) 0.2494(2) 0.5881(2) 0.0405(6) Uani 1 1 d . . . . .
H54 H 0.7914 0.2076 0.6251 0.049 Uiso 1 1 calc R U . . .
C55 C 0.7460(2) 0.3502(2) 0.5727(2) 0.0424(6) Uani 1 1 d . . . . .
C56 C 0.6814(2) 0.40969(19) 0.5152(2) 0.0389(6) Uani 1 1 d . . . . .
H56 H 0.6818 0.4796 0.5010 0.047 Uiso 1 1 calc R U . . .
C57 C 0.61587(19) 0.36996(18) 0.47759(19) 0.0348(5) Uani 1 1 d . . . . .
C58 C 0.6937(2) 0.0957(2) 0.5718(2) 0.0462(7) Uani 1 1 d . . . . .
H58A H 0.7537 0.0723 0.5983 0.069 Uiso 1 1 calc R U . . .
H58B H 0.6969 0.0821 0.5095 0.069 Uiso 1 1 calc R U . . .
H58C H 0.6378 0.0611 0.6207 0.069 Uiso 1 1 calc R U . . .
C59 C 0.8137(3) 0.3934(3) 0.6164(3) 0.0632(9) Uani 1 1 d . . . . .
H59A H 0.8079 0.3561 0.6880 0.095 Uiso 1 1 calc R U . . .
H59B H 0.7964 0.4633 0.6066 0.095 Uiso 1 1 calc R U . . .
H59C H 0.8809 0.3889 0.5830 0.095 Uiso 1 1 calc R U . . .
C60 C 0.5510(2) 0.44329(18) 0.4137(2) 0.0380(6) Uani 1 1 d . . . . .
H60A H 0.4845 0.4391 0.4515 0.057 Uiso 1 1 calc R U . . .
H60B H 0.5511 0.4274 0.3532 0.057 Uiso 1 1 calc R U . . .
H60C H 0.5755 0.5108 0.3952 0.057 Uiso 1 1 calc R U . . .
C61 C 0.41770(19) 0.26778(18) 0.4828(2) 0.0374(6) Uani 1 1 d . . . . .
C62 C 0.3817(2) 0.27265(19) 0.5796(2) 0.0414(6) Uani 1 1 d . . . . .
C63 C 0.2852(2) 0.3003(2) 0.6051(3) 0.0529(8) Uani 1 1 d . . . . .
H63 H 0.2631 0.3029 0.6703 0.064 Uiso 1 1 calc R U . . .
C64 C 0.2206(2) 0.3239(2) 0.5397(3) 0.0602(9) Uani 1 1 d . . . . .
C65 C 0.2551(2) 0.3197(2) 0.4456(3) 0.0577(9) Uani 1 1 d . . . . .
H65 H 0.2121 0.3361 0.3988 0.069 Uiso 1 1 calc R U . . .
C66 C 0.3512(2) 0.2920(2) 0.4163(2) 0.0475(7) Uani 1 1 d . . . . .
C67 C 0.4426(2) 0.2492(2) 0.6605(2) 0.0454(7) Uani 1 1 d . . . . .
H67A H 0.4841 0.3061 0.6477 0.068 Uiso 1 1 calc R U . . .
H67B H 0.4834 0.1906 0.6606 0.068 Uiso 1 1 calc R U . . .
H67C H 0.3997 0.2358 0.7255 0.068 Uiso 1 1 calc R U . . .
C68 C 0.1157(3) 0.3500(3) 0.5713(4) 0.0910(15) Uani 1 1 d . . . . .
H68A H 0.0884 0.3000 0.6349 0.136 Uiso 1 1 calc R U . . .
H68B H 0.0782 0.3516 0.5202 0.136 Uiso 1 1 calc R U . . .
H68C H 0.1125 0.4155 0.5792 0.136 Uiso 1 1 calc R U . . .
C69 C 0.3781(3) 0.2886(3) 0.3119(3) 0.0719(11) Uani 1 1 d . . . . .
H69A H 0.3211 0.3065 0.2789 0.108 Uiso 1 1 calc R U . . .
H69B H 0.4000 0.2214 0.3145 0.108 Uiso 1 1 calc R U . . .
H69C H 0.4306 0.3359 0.2741 0.108 Uiso 1 1 calc R U . . .
B1 B 0.9994(2) 0.06335(19) 0.2753(2) 0.0309(5) Uani 1 1 d . . . . .
B2 B 0.5268(2) 0.2215(2) 0.4618(2) 0.0345(6) Uani 1 1 d . . . . .
N1 N 0.96398(15) 0.17636(14) 0.27685(15) 0.0320(4) Uani 1 1 d . . . . .
N2 N 0.94021(16) 0.25926(15) 0.20943(15) 0.0343(5) Uani 1 1 d . . . . .
N3 N 0.90398(16) 0.31846(15) 0.26194(15) 0.0354(5) Uani 1 1 d . . . . .
N4 N 0.57489(16) 0.23490(15) 0.34438(16) 0.0354(5) Uani 1 1 d . . . . .
N5 N 0.61455(17) 0.31002(15) 0.26717(16) 0.0384(5) Uani 1 1 d . . . . .
N6 N 0.65431(18) 0.26868(16) 0.19863(16) 0.0390(5) Uani 1 1 d . . . . .
C31 C 0.4112(9) 0.6877(8) 0.1345(11) 0.121(5) Uani 0.5 1 d . . P . .
H31A H 0.3995 0.7294 0.1777 0.146 Uiso 0.5 1 calc R U P . .
H31B H 0.3482 0.6803 0.1163 0.146 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.4488(3) 0.5762(3) 0.1998(3) 0.1366(13) Uani 0.5 1 d . . P . .
Cl2 Cl 0.4891(4) 0.7484(4) 0.0287(5) 0.207(3) Uani 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.394(3) 2_756 ?
C1 C2 1.408(3) . ?
C1 B1 1.646(3) . ?
C2 C3 1.394(3) . ?
C2 C4 1.457(3) . ?
C3 C1 1.394(3) 2_756 ?
C3 H3 0.9500 . ?
C4 N1 1.357(3) . ?
C4 C5 1.366(4) . ?
C5 N3 1.360(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.374(4) . ?
C6 C11 1.375(4) . ?
C6 N3 1.439(3) . ?
C7 C8 1.392(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.371(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(4) . ?
C9 C12 1.512(4) . ?
C10 C11 1.379(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.412(4) . ?
C13 C14 1.415(4) . ?
C13 B1 1.637(4) . ?
C14 C15 1.397(4) . ?
C14 C19 1.515(4) . ?
C15 C16 1.389(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.365(5) . ?
C16 C20 1.511(4) . ?
C17 C18 1.396(4) . ?
C17 H17 0.9500 . ?
C18 C21 1.511(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.413(3) . ?
C22 C27 1.422(3) . ?
C22 B1 1.636(4) . ?
C23 C24 1.393(4) . ?
C23 C28 1.514(4) . ?
C24 C25 1.382(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(4) . ?
C25 C29 1.510(4) . ?
C26 C27 1.386(4) . ?
C26 H26 0.9500 . ?
C27 C30 1.514(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C40 C42 1.391(4) 2_656 ?
C40 C41 1.410(4) . ?
C40 B2 1.642(4) . ?
C41 C42 1.396(3) . ?
C41 C43 1.459(4) . ?
C42 C40 1.390(4) 2_656 ?
C42 H42 0.9500 . ?
C43 N4 1.361(3) . ?
C43 C44 1.367(4) . ?
C44 N6 1.358(3) . ?
C44 H44 0.9500 . ?
C45 C50 1.355(4) . ?
C45 C46 1.388(4) . ?
C45 N6 1.441(3) . ?
C46 C47 1.381(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.403(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.371(4) . ?
C48 C51 1.517(4) . ?
C49 C50 1.394(4) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.417(4) . ?
C52 C57 1.420(3) . ?
C52 B2 1.636(4) . ?
C53 C54 1.394(4) . ?
C53 C58 1.514(4) . ?
C54 C55 1.383(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.388(4) . ?
C55 C59 1.507(4) . ?
C56 C57 1.395(4) . ?
C56 H56 0.9500 . ?
C57 C60 1.516(4) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C66 1.409(4) . ?
C61 C62 1.420(4) . ?
C61 B2 1.635(4) . ?
C62 C63 1.396(4) . ?
C62 C67 1.511(4) . ?
C63 C64 1.375(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.377(6) . ?
C64 C68 1.512(5) . ?
C65 C66 1.402(4) . ?
C65 H65 0.9500 . ?
C66 C69 1.504(5) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
B1 N1 1.664(3) . ?
B2 N4 1.655(4) . ?
N1 N2 1.320(3) . ?
N2 N3 1.338(3) . ?
N4 N5 1.318(3) . ?
N5 N6 1.339(3) . ?
C31 Cl1 1.658(11) . ?
C31 Cl2 1.694(15) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C1 C2 116.4(2) 2_756 . ?
C3 C1 B1 130.5(2) 2_756 . ?
C2 C1 B1 112.9(2) . . ?
C3 C2 C1 124.4(2) . . ?
C3 C2 C4 126.6(2) . . ?
C1 C2 C4 109.0(2) . . ?
C1 C3 C2 119.2(2) 2_756 . ?
C1 C3 H3 120.4 2_756 . ?
C2 C3 H3 120.4 . . ?
N1 C4 C5 106.6(2) . . ?
N1 C4 C2 111.2(2) . . ?
C5 C4 C2 142.2(2) . . ?
N3 C5 C4 104.8(2) . . ?
N3 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
C7 C6 C11 120.6(2) . . ?
C7 C6 N3 120.8(2) . . ?
C11 C6 N3 118.6(2) . . ?
C6 C7 C8 118.8(3) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 118.2(3) . . ?
C8 C9 C12 121.7(3) . . ?
C10 C9 C12 120.1(3) . . ?
C11 C10 C9 121.3(3) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C6 C11 C10 119.5(3) . . ?
C6 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 116.4(2) . . ?
C18 C13 B1 124.9(2) . . ?
C14 C13 B1 118.0(2) . . ?
C15 C14 C13 120.4(3) . . ?
C15 C14 C19 116.3(3) . . ?
C13 C14 C19 123.3(2) . . ?
C16 C15 C14 122.4(3) . . ?
C16 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C17 C16 C15 117.1(3) . . ?
C17 C16 C20 121.6(4) . . ?
C15 C16 C20 121.3(4) . . ?
C16 C17 C18 122.6(3) . . ?
C16 C17 H17 118.7 . . ?
C18 C17 H17 118.7 . . ?
C17 C18 C13 120.9(3) . . ?
C17 C18 C21 116.2(3) . . ?
C13 C18 C21 122.9(3) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C27 116.4(2) . . ?
C23 C22 B1 124.5(2) . . ?
C27 C22 B1 119.1(2) . . ?
C24 C23 C22 120.5(2) . . ?
C24 C23 C28 116.0(2) . . ?
C22 C23 C28 123.5(2) . . ?
C25 C24 C23 122.7(2) . . ?
C25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C24 C25 C26 117.0(2) . . ?
C24 C25 C29 121.6(3) . . ?
C26 C25 C29 121.3(3) . . ?
C27 C26 C25 122.3(2) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C26 C27 C22 121.0(2) . . ?
C26 C27 C30 116.5(2) . . ?
C22 C27 C30 122.5(2) . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C42 C40 C41 116.2(2) 2_656 . ?
C42 C40 B2 130.5(2) 2_656 . ?
C41 C40 B2 113.1(2) . . ?
C42 C41 C40 124.4(2) . . ?
C42 C41 C43 126.9(2) . . ?
C40 C41 C43 108.6(2) . . ?
C40 C42 C41 119.4(2) 2_656 . ?
C40 C42 H42 120.3 2_656 . ?
C41 C42 H42 120.3 . . ?
N4 C43 C44 106.4(2) . . ?
N4 C43 C41 110.9(2) . . ?
C44 C43 C41 142.7(2) . . ?
N6 C44 C43 104.9(2) . . ?
N6 C44 H44 127.6 . . ?
C43 C44 H44 127.6 . . ?
C50 C45 C46 122.2(3) . . ?
C50 C45 N6 118.5(2) . . ?
C46 C45 N6 119.2(3) . . ?
C47 C46 C45 117.9(3) . . ?
C47 C46 H46 121.0 . . ?
C45 C46 H46 121.0 . . ?
C46 C47 C48 121.6(3) . . ?
C46 C47 H47 119.2 . . ?
C48 C47 H47 119.2 . . ?
C49 C48 C47 117.8(3) . . ?
C49 C48 C51 121.1(3) . . ?
C47 C48 C51 121.1(3) . . ?
C48 C49 C50 121.7(3) . . ?
C48 C49 H49 119.1 . . ?
C50 C49 H49 119.1 . . ?
C45 C50 C49 118.7(3) . . ?
C45 C50 H50 120.6 . . ?
C49 C50 H50 120.6 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C53 C52 C57 116.5(2) . . ?
C53 C52 B2 124.2(2) . . ?
C57 C52 B2 119.3(2) . . ?
C54 C53 C52 120.5(2) . . ?
C54 C53 C58 116.2(2) . . ?
C52 C53 C58 123.3(2) . . ?
C55 C54 C53 122.7(3) . . ?
C55 C54 H54 118.7 . . ?
C53 C54 H54 118.7 . . ?
C54 C55 C56 117.3(3) . . ?
C54 C55 C59 121.3(3) . . ?
C56 C55 C59 121.5(3) . . ?
C55 C56 C57 121.9(2) . . ?
C55 C56 H56 119.0 . . ?
C57 C56 H56 119.0 . . ?
C56 C57 C52 121.0(2) . . ?
C56 C57 C60 116.7(2) . . ?
C52 C57 C60 122.4(2) . . ?
C53 C58 H58A 109.5 . . ?
C53 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C53 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C55 C59 H59A 109.5 . . ?
C55 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C55 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C66 C61 C62 116.4(3) . . ?
C66 C61 B2 124.9(3) . . ?
C62 C61 B2 118.2(2) . . ?
C63 C62 C61 120.4(3) . . ?
C63 C62 C67 115.9(3) . . ?
C61 C62 C67 123.7(2) . . ?
C64 C63 C62 122.8(3) . . ?
C64 C63 H63 118.6 . . ?
C62 C63 H63 118.6 . . ?
C63 C64 C65 117.1(3) . . ?
C63 C64 C68 121.2(4) . . ?
C65 C64 C68 121.7(4) . . ?
C64 C65 C66 122.4(3) . . ?
C64 C65 H65 118.8 . . ?
C66 C65 H65 118.8 . . ?
C65 C66 C61 120.8(3) . . ?
C65 C66 C69 116.6(3) . . ?
C61 C66 C69 122.6(3) . . ?
C62 C67 H67A 109.5 . . ?
C62 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C62 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C64 C68 H68A 109.5 . . ?
C64 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C64 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C66 C69 H69A 109.5 . . ?
C66 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C66 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C22 B1 C13 116.4(2) . . ?
C22 B1 C1 121.6(2) . . ?
C13 B1 C1 104.25(19) . . ?
C22 B1 N1 102.47(18) . . ?
C13 B1 N1 117.1(2) . . ?
C1 B1 N1 93.44(18) . . ?
C61 B2 C52 115.4(2) . . ?
C61 B2 C40 105.3(2) . . ?
C52 B2 C40 121.7(2) . . ?
C61 B2 N4 117.2(2) . . ?
C52 B2 N4 102.4(2) . . ?
C40 B2 N4 93.48(19) . . ?
N2 N1 C4 111.9(2) . . ?
N2 N1 B1 134.43(19) . . ?
C4 N1 B1 113.04(19) . . ?
N1 N2 N3 104.42(19) . . ?
N2 N3 C5 112.3(2) . . ?
N2 N3 C6 121.0(2) . . ?
C5 N3 C6 126.7(2) . . ?
N5 N4 C43 112.0(2) . . ?
N5 N4 B2 133.9(2) . . ?
C43 N4 B2 113.3(2) . . ?
N4 N5 N6 104.35(19) . . ?
N5 N6 C44 112.4(2) . . ?
N5 N6 C45 119.5(2) . . ?
C44 N6 C45 128.0(2) . . ?
Cl1 C31 Cl2 115.0(8) . . ?
Cl1 C31 H31A 108.5 . . ?
Cl2 C31 H31A 108.5 . . ?
Cl1 C31 H31B 108.5 . . ?
Cl2 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?

_refine_diff_density_max         0.608
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.052

