# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_Compound_5a
_database_code_depnum_ccdc_archive 'CCDC 1587634'
_audit_update_record             
;
2018-01-14 deposited with the CCDC.
2018-01-31 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         'C38 H34 B2 F2 N4 O'
_chemical_formula_sum            'C38 H34 B2 F2 N4 O'
_chemical_formula_weight         622.31

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'

_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, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   23.237(2)
_cell_length_b                   10.5234(10)
_cell_length_c                   12.0981(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2958.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    99(2)
_cell_measurement_reflns_used    9674

_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      27.73

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.093
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9656
_exptl_absorpt_correction_T_max  0.9954
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9674
_diffrn_reflns_av_unetI/netI     0.1109
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.124
_diffrn_reflns_theta_max         27.734
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_point_group_measured_fraction_full 0.923
_reflns_number_total             3154
_reflns_number_gt                2055
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_max     0.766
_reflns_Friedel_fraction_full    0.839

_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       'SMART (Siemens, 1995)'

_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'


_computing_publication_material  'SHELXTL (Sheldrick, 2008)'


_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)+(0.0687P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3154
_refine_ls_number_parameters     223
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1395
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_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 0.40482(11) 0.2408(2) 0.5877(2) 0.0288(7) Uani 1 1 d . . . . .
O O 0.5000 0.2590(4) 0.6321(3) 0.0221(10) Uani 1 2 d S T P . .
N1 N 0.42853(16) 0.2067(3) 0.7770(3) 0.0213(9) Uani 1 1 d . . . . .
N2 N 0.43007(16) 0.4251(3) 0.6928(3) 0.0220(9) Uani 1 1 d . . . . .
C1 C 0.5000 0.0197(6) 0.7823(5) 0.0223(14) Uani 1 2 d S T P . .
C8 C 0.35870(18) 0.3700(4) 0.8316(4) 0.0237(10) Uani 1 1 d . . . . .
C10 C 0.2618(2) 0.3402(4) 0.9206(4) 0.0295(11) Uani 1 1 d . . . . .
H10 H 0.2549 0.2714 0.8742 0.035 Uiso 1 1 calc R U . . .
C9 C 0.31285(18) 0.4097(4) 0.9090(4) 0.0228(10) Uani 1 1 d . . . . .
C19 C 0.44735(19) 0.5306(4) 0.6373(4) 0.0234(11) Uani 1 1 d . . . . .
C11 C 0.2212(2) 0.3722(5) 1.0001(4) 0.0311(12) Uani 1 1 d . . . . .
H11 H 0.1875 0.3249 1.0060 0.037 Uiso 1 1 calc R U . . .
C4 C 0.44592(19) 0.0925(4) 0.8179(4) 0.0217(10) Uani 1 1 d . . . . .
C2 C 0.5000 -0.0142(6) 0.6587(6) 0.0284(15) Uani 1 2 d S T P . .
H2A H 0.5347 -0.0595 0.6410 0.043 Uiso 0.5 1 calc R U P . .
H2B H 0.4673 -0.0667 0.6424 0.043 Uiso 0.5 1 calc R U P . .
H2C H 0.4981 0.0622 0.6157 0.043 Uiso 1 2 calc R U P . .
C17 C 0.3710(2) 0.5870(4) 0.7419(4) 0.0280(11) Uani 1 1 d . . . . .
H17 H 0.3416 0.6334 0.7749 0.034 Uiso 1 1 calc R U . . .
C18 C 0.41061(19) 0.6323(4) 0.6674(4) 0.0256(11) Uani 1 1 d . . . . .
H18 H 0.4129 0.7153 0.6412 0.031 Uiso 1 1 calc R U . . .
C7 C 0.3803(2) 0.2459(4) 0.8408(4) 0.0256(11) Uani 1 1 d . . . . .
C22 C 0.5000 0.6744(7) 0.5113(6) 0.0275(16) Uani 1 2 d S T P . .
H22A H 0.4672 0.6834 0.4638 0.041 Uiso 0.5 1 calc R U P . .
H22B H 0.4983 0.7370 0.5690 0.041 Uiso 1 2 calc R U P . .
H22C H 0.5346 0.6861 0.4691 0.041 Uiso 0.5 1 calc R U P . .
C6 C 0.3696(2) 0.1522(4) 0.9202(4) 0.0246(10) Uani 1 1 d . . . . .
H6 H 0.3406 0.1539 0.9733 0.029 Uiso 1 1 calc R U . . .
C15 C 0.3209(2) 0.5152(4) 0.9768(4) 0.0262(11) Uani 1 1 d . . . . .
H15 H 0.3536 0.5651 0.9682 0.031 Uiso 1 1 calc R U . . .
C12 C 0.2304(2) 0.4746(4) 1.0711(4) 0.0292(11) Uani 1 1 d . . . . .
C3 C 0.5000 -0.1104(6) 0.8432(6) 0.0275(16) Uani 1 2 d S T P . .
H3A H 0.5335 -0.1579 0.8223 0.041 Uiso 0.5 1 calc R U P . .
H3B H 0.5004 -0.0964 0.9216 0.041 Uiso 1 2 calc R U P . .
H3C H 0.4661 -0.1572 0.8233 0.041 Uiso 0.5 1 calc R U P . .
C5 C 0.40955(19) 0.0570(4) 0.9055(4) 0.0259(10) Uani 1 1 d . . . . .
H5 H 0.4121 -0.0177 0.9464 0.031 Uiso 1 1 calc R U . . .
C14 C 0.2804(2) 0.5469(5) 1.0577(4) 0.0317(12) Uani 1 1 d . . . . .
H14 H 0.2868 0.6168 1.1031 0.038 Uiso 1 1 calc R U . . .
C20 C 0.5000 0.5425(6) 0.5621(5) 0.0240(15) Uani 1 2 d S T P . .
B B 0.4444(2) 0.2794(5) 0.6681(4) 0.0233(12) Uani 1 1 d . . . . .
C13 C 0.1886(2) 0.5058(6) 1.1636(5) 0.0425(13) Uani 1 1 d . . . . .
H13A H 0.2021 0.5789 1.2033 0.064 Uiso 1 1 calc R U . . .
H13B H 0.1513 0.5234 1.1329 0.064 Uiso 1 1 calc R U . . .
H13C H 0.1859 0.4347 1.2131 0.064 Uiso 1 1 calc R U . . .
C21 C 0.5000 0.4520(6) 0.4595(5) 0.0254(15) Uani 1 2 d S T P . .
H21A H 0.5000 0.3652 0.4840 0.038 Uiso 1 2 calc R U P . .
H21B H 0.4663 0.4676 0.4157 0.038 Uiso 0.5 1 calc R U P . .
H21C H 0.5337 0.4676 0.4157 0.038 Uiso 0.5 1 calc R U P . .
C16 C 0.38326(18) 0.4575(4) 0.7590(4) 0.0230(10) 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 B 1.400(6) . ?
O B 1.379(6) . ?
O B 1.379(6) 3_655 ?
N1 C4 1.360(5) . ?
N1 C7 1.421(6) . ?
N1 B 1.569(6) . ?
N2 C19 1.358(6) . ?
N2 C16 1.393(6) . ?
N2 B 1.598(6) . ?
C1 C4 1.533(6) . ?
C1 C4 1.533(6) 3_655 ?
C1 C2 1.537(9) . ?
C1 C3 1.555(9) . ?
C8 C16 1.395(6) . ?
C8 C7 1.404(6) . ?
C8 C9 1.478(6) . ?
C10 C11 1.388(7) . ?
C10 C9 1.402(6) . ?
C9 C15 1.393(6) . ?
C19 C18 1.417(6) . ?
C19 C20 1.530(6) . ?
C11 C12 1.395(7) . ?
C4 C5 1.407(6) . ?
C17 C18 1.373(7) . ?
C17 C16 1.408(6) . ?
C7 C6 1.399(6) . ?
C22 C20 1.518(9) . ?
C6 C5 1.378(6) . ?
C15 C14 1.397(7) . ?
C12 C14 1.399(7) . ?
C12 C13 1.518(7) . ?
C20 C19 1.530(6) 3_655 ?
C20 C21 1.565(9) . ?

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
B O B 138.8(5) . 3_655 ?
C4 N1 C7 107.1(4) . . ?
C4 N1 B 131.8(4) . . ?
C7 N1 B 120.0(4) . . ?
C19 N2 C16 108.3(4) . . ?
C19 N2 B 129.1(4) . . ?
C16 N2 B 120.4(4) . . ?
C4 C1 C4 110.1(5) . 3_655 ?
C4 C1 C2 112.9(3) . . ?
C4 C1 C2 112.9(3) 3_655 . ?
C4 C1 C3 107.9(4) . . ?
C4 C1 C3 107.9(4) 3_655 . ?
C2 C1 C3 104.8(5) . . ?
C16 C8 C7 121.1(4) . . ?
C16 C8 C9 120.5(4) . . ?
C7 C8 C9 118.1(4) . . ?
C11 C10 C9 121.2(5) . . ?
C15 C9 C10 118.0(4) . . ?
C15 C9 C8 120.1(4) . . ?
C10 C9 C8 121.8(4) . . ?
N2 C19 C18 108.2(4) . . ?
N2 C19 C20 126.7(4) . . ?
C18 C19 C20 124.9(4) . . ?
C10 C11 C12 120.6(4) . . ?
N1 C4 C5 109.3(4) . . ?
N1 C4 C1 125.6(4) . . ?
C5 C4 C1 124.8(4) . . ?
C18 C17 C16 107.3(4) . . ?
C17 C18 C19 108.0(4) . . ?
C6 C7 C8 130.2(4) . . ?
C6 C7 N1 108.0(4) . . ?
C8 C7 N1 120.7(4) . . ?
C5 C6 C7 107.7(4) . . ?
C9 C15 C14 120.8(4) . . ?
C11 C12 C14 118.5(5) . . ?
C11 C12 C13 121.5(4) . . ?
C14 C12 C13 120.0(5) . . ?
C6 C5 C4 108.0(4) . . ?
C15 C14 C12 120.7(5) . . ?
C22 C20 C19 108.4(4) . 3_655 ?
C22 C20 C19 108.4(4) . . ?
C19 C20 C19 106.2(5) 3_655 . ?
C22 C20 C21 103.6(5) . . ?
C19 C20 C21 115.0(3) 3_655 . ?
C19 C20 C21 115.0(3) . . ?
O B F1 110.6(4) . . ?
O B N1 114.2(4) . . ?
F1 B N1 106.7(4) . . ?
O B N2 113.8(4) . . ?
F1 B N2 105.7(4) . . ?
N1 B N2 105.2(4) . . ?
N2 C16 C8 121.3(4) . . ?
N2 C16 C17 108.1(4) . . ?
C8 C16 C17 130.5(4) . . ?

_refine_diff_density_max         0.303
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_Compound_4a
_database_code_depnum_ccdc_archive 'CCDC 1587636'
_audit_update_record             
;
2018-01-14 deposited with the CCDC.
2018-01-31 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         'C38 H36 B F2 N4, B F4, C H Cl3, 0.5(C H Cl3)'
_chemical_formula_sum            'C39.50 H37.50 B2 Cl4.50 F6 N4'
_chemical_formula_weight         863.38

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_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+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'

_cell_length_a                   21.5460(9)
_cell_length_b                   31.9600(12)
_cell_length_c                   11.6400(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8015.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    99(2)
_cell_measurement_reflns_used    109808
_cell_measurement_theta_min      1.274
_cell_measurement_theta_max      27.950

_exptl_crystal_description       needle
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_F_000             3544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.392
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.815050
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            109808
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_av_R_equivalents  0.1654
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.274
_diffrn_reflns_theta_max         27.950
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9554
_reflns_number_gt                4507
_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       'SMART (Siemens, 1995)'
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_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)+(0.0704P)²+27.3201P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9554
_refine_ls_number_parameters     544
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.1827
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.2183
_refine_ls_wR_factor_gt          0.1569
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      1.007
_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 0.51068(19) 0.69069(12) 0.5063(4) 0.0196(9) Uani 1 1 d . . . . .
C2 C 0.57133(19) 0.68465(12) 0.4632(4) 0.0226(9) Uani 1 1 d . . . . .
H2 H 0.6036 0.7040 0.4668 0.027 Uiso 1 1 calc R U . . .
C3 C 0.5747(2) 0.64538(13) 0.4149(4) 0.0254(10) Uani 1 1 d . . . . .
H3 H 0.6097 0.6330 0.3826 0.031 Uiso 1 1 calc R U . . .
C4 C 0.51532(19) 0.62762(12) 0.4238(4) 0.0208(9) Uani 1 1 d . . . . .
C5 C 0.4942(2) 0.58679(12) 0.3729(4) 0.0243(10) Uani 1 1 d . . . . .
C6 C 0.4857(2) 0.59231(14) 0.2405(4) 0.0297(10) Uani 1 1 d . . . . .
H6A H 0.4738 0.5661 0.2070 0.045 Uiso 1 1 calc R U . . .
H6B H 0.5241 0.6015 0.2071 0.045 Uiso 1 1 calc R U . . .
H6C H 0.4540 0.6128 0.2260 0.045 Uiso 1 1 calc R U . . .
C7 C 0.5444(2) 0.55318(13) 0.3947(5) 0.0339(12) Uani 1 1 d . . . . .
H7A H 0.5505 0.5498 0.4759 0.051 Uiso 1 1 calc R U . . .
H7B H 0.5827 0.5618 0.3597 0.051 Uiso 1 1 calc R U . . .
H7C H 0.5313 0.5271 0.3620 0.051 Uiso 1 1 calc R U . . .
C8 C 0.43359(19) 0.57228(12) 0.4226(4) 0.0216(9) Uani 1 1 d . . . . .
C9 C 0.4078(2) 0.53218(12) 0.4087(4) 0.0242(10) Uani 1 1 d . . . . .
H9 H 0.4267 0.5092 0.3745 0.029 Uiso 1 1 calc R U . . .
C10 C 0.3496(2) 0.53369(12) 0.4552(4) 0.0243(10) Uani 1 1 d . . . . .
H10 H 0.3212 0.5118 0.4561 0.029 Uiso 1 1 calc R U . . .
C11 C 0.33959(19) 0.57417(12) 0.5020(4) 0.0204(9) Uani 1 1 d . . . . .
C12 C 0.28637(19) 0.58358(12) 0.5671(3) 0.0190(9) Uani 1 1 d . . . . .
C13 C 0.23006(18) 0.55977(12) 0.5359(4) 0.0206(9) Uani 1 1 d . . . . .
C14 C 0.21448(19) 0.55495(12) 0.4198(4) 0.0205(9) Uani 1 1 d . . . . .
H14 H 0.2387 0.5679 0.3640 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1640(2) 0.53130(12) 0.3864(4) 0.0243(10) Uani 1 1 d . . . . .
H15 H 0.1545 0.5288 0.3088 0.029 Uiso 1 1 calc R U . . .
C16 C 0.1272(2) 0.51121(13) 0.4672(4) 0.0270(10) Uani 1 1 d . . . . .
C17 C 0.1411(2) 0.51632(13) 0.5831(4) 0.0276(10) Uani 1 1 d . . . . .
H17 H 0.1165 0.5034 0.6383 0.033 Uiso 1 1 calc R U . . .
C18 C 0.1917(2) 0.54067(13) 0.6173(4) 0.0261(10) Uani 1 1 d . . . . .
H18 H 0.1999 0.5442 0.6951 0.031 Uiso 1 1 calc R U . . .
C19 C 0.0740(2) 0.48398(15) 0.4278(4) 0.0353(12) Uani 1 1 d . . . . .
H19A H 0.0449 0.5006 0.3851 0.053 Uiso 1 1 calc R U . . .
H19B H 0.0536 0.4721 0.4935 0.053 Uiso 1 1 calc R U . . .
H19C H 0.0896 0.4619 0.3798 0.053 Uiso 1 1 calc R U . . .
C20 C 0.28229(19) 0.61152(11) 0.6617(3) 0.0186(9) Uani 1 1 d . . . . .
C21 C 0.22983(19) 0.62984(12) 0.7112(4) 0.0208(9) Uani 1 1 d . . . . .
H21 H 0.1890 0.6257 0.6881 0.025 Uiso 1 1 calc R U . . .
C22 C 0.2494(2) 0.65517(12) 0.8004(4) 0.0219(9) Uani 1 1 d . . . . .
H22 H 0.2241 0.6716 0.8470 0.026 Uiso 1 1 calc R U . . .
C23 C 0.3140(2) 0.65169(12) 0.8082(4) 0.0208(9) Uani 1 1 d . . . . .
C24 C 0.3586(2) 0.67469(13) 0.8872(4) 0.0231(9) Uani 1 1 d . . . . .
C25 C 0.3211(2) 0.69940(13) 0.9765(4) 0.0279(10) Uani 1 1 d . . . . .
H25A H 0.2976 0.6803 1.0230 0.042 Uiso 1 1 calc R U . . .
H25B H 0.2934 0.7183 0.9379 0.042 Uiso 1 1 calc R U . . .
H25C H 0.3490 0.7150 1.0245 0.042 Uiso 1 1 calc R U . . .
C26 C 0.4031(2) 0.64443(13) 0.9479(4) 0.0264(10) Uani 1 1 d . . . . .
H26A H 0.3797 0.6253 0.9945 0.040 Uiso 1 1 calc R U . . .
H26B H 0.4312 0.6600 0.9956 0.040 Uiso 1 1 calc R U . . .
H26C H 0.4263 0.6290 0.8915 0.040 Uiso 1 1 calc R U . . .
C27 C 0.39298(19) 0.70539(12) 0.8106(4) 0.0208(9) Uani 1 1 d . . . . .
C28 C 0.38710(19) 0.74910(13) 0.8049(4) 0.0222(9) Uani 1 1 d . . . . .
H28 H 0.3624 0.7657 0.8520 0.027 Uiso 1 1 calc R U . . .
C29 C 0.42486(19) 0.76297(12) 0.7163(4) 0.0220(9) Uani 1 1 d . . . . .
H29 H 0.4304 0.7907 0.6941 0.026 Uiso 1 1 calc R U . . .
C30 C 0.45340(19) 0.72772(12) 0.6653(4) 0.0205(9) Uani 1 1 d . . . . .
C31 C 0.49525(18) 0.72577(12) 0.5730(4) 0.0202(9) Uani 1 1 d . . . . .
C32 C 0.52949(19) 0.76467(12) 0.5450(4) 0.0214(9) Uani 1 1 d . . . . .
C33 C 0.5560(2) 0.79002(13) 0.6300(4) 0.0252(10) Uani 1 1 d . . . . .
H33 H 0.5508 0.7831 0.7070 0.030 Uiso 1 1 calc R U . . .
C34 C 0.5898(2) 0.82525(14) 0.6006(4) 0.0295(10) Uani 1 1 d . . . . .
H34 H 0.6074 0.8414 0.6586 0.035 Uiso 1 1 calc R U . . .
C35 C 0.5983(2) 0.83719(13) 0.4872(4) 0.0287(10) Uani 1 1 d . . . . .
C36 C 0.57108(19) 0.81247(13) 0.4026(4) 0.0261(10) Uani 1 1 d . . . . .
H36 H 0.5753 0.8201 0.3259 0.031 Uiso 1 1 calc R U . . .
C37 C 0.53792(19) 0.77682(12) 0.4298(4) 0.0218(9) Uani 1 1 d . . . . .
H37 H 0.5209 0.7606 0.3713 0.026 Uiso 1 1 calc R U . . .
C38 C 0.6353(2) 0.87558(15) 0.4561(5) 0.0414(13) Uani 1 1 d . . . . .
H38A H 0.6111 0.8931 0.4064 0.062 Uiso 1 1 calc R U . . .
H38B H 0.6727 0.8674 0.4174 0.062 Uiso 1 1 calc R U . . .
H38C H 0.6457 0.8907 0.5247 0.062 Uiso 1 1 calc R U . . .
N1 N 0.47620(15) 0.65387(10) 0.4815(3) 0.0194(7) Uani 1 1 d . . . . .
N2 N 0.39409(15) 0.59792(10) 0.4799(3) 0.0185(7) Uani 1 1 d . . . . .
N3 N 0.33252(16) 0.62512(10) 0.7250(3) 0.0194(7) Uani 1 1 d . . . . .
H3A H 0.3703 0.6177 0.7131 0.023 Uiso 1 1 calc R U . . .
N4 N 0.43294(15) 0.69335(10) 0.7278(3) 0.0202(8) Uani 1 1 d . . . . .
H4 H 0.4442 0.6679 0.7154 0.024 Uiso 1 1 calc R U . . .
B1 B 0.4043(2) 0.64673(13) 0.4639(4) 0.0187(10) Uani 1 1 d . . . . .
F1 F 0.39052(10) 0.65594(7) 0.3494(2) 0.0211(5) Uani 1 1 d . . . . .
F2 F 0.36830(10) 0.67034(6) 0.53477(19) 0.0204(5) Uani 1 1 d . . . . .
B2 B 0.5076(2) 0.58103(14) 0.7308(5) 0.0294(12) Uani 1 1 d D . . . .
F3 F 0.51296(18) 0.57491(13) 0.8531(3) 0.0807(12) Uani 1 1 d . . . . .
F4 F 0.45983(18) 0.60714(13) 0.7104(3) 0.0322(14) Uani 0.684(9) 1 d D U P A 1
F5 F 0.5613(2) 0.6009(3) 0.6971(5) 0.096(3) Uani 0.684(9) 1 d D U P A 1
F6 F 0.4996(5) 0.54344(17) 0.6869(6) 0.109(4) Uani 0.684(9) 1 d D U P A 1
F4A F 0.4466(4) 0.5721(4) 0.7131(9) 0.055(4) Uani 0.316(9) 1 d D U P A 2
F5A F 0.5170(6) 0.6215(2) 0.7161(9) 0.055(4) Uani 0.316(9) 1 d D U P A 2
F6A F 0.5456(6) 0.5594(4) 0.6733(15) 0.085(5) Uani 0.316(9) 1 d D U P A 2
Cl1 Cl 0.71480(11) 0.55689(5) 0.72236(15) 0.0806(6) Uani 1 1 d . . . . .
Cl2 Cl 0.71279(6) 0.57799(4) 0.48244(13) 0.0467(4) Uani 1 1 d . . . . .
Cl3 Cl 0.71986(11) 0.64376(5) 0.65146(19) 0.0960(8) Uani 1 1 d . . . . .
C39 C 0.6911(3) 0.59378(16) 0.6212(5) 0.0539(16) Uani 1 1 d . . . . .
H39 H 0.6456 0.5952 0.6236 0.065 Uiso 1 1 calc R U . . .
Cl4 Cl 0.69045(9) 0.73106(9) 0.2728(2) 0.1117(9) Uani 1 1 d D . . . .
Cl5 Cl 0.7500 0.7500 0.4835(3) 0.179(2) Uani 1 2 d DS T P . .
C40 C 0.7356(5) 0.7669(3) 0.3488(8) 0.070(4) Uani 0.5 1 d D . P B -1
H40 H 0.7158 0.7945 0.3500 0.084 Uiso 0.5 1 calc R U 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
C1 C31 1.404(6) . ?
C1 C2 1.413(6) . ?
C1 N1 1.421(5) . ?
C2 C3 1.377(6) . ?
C3 C4 1.404(6) . ?
C4 N1 1.366(5) . ?
C4 C5 1.503(6) . ?
C5 C8 1.502(6) . ?
C5 C7 1.546(6) . ?
C5 C6 1.562(6) . ?
C8 N2 1.356(5) . ?
C8 C9 1.406(6) . ?
C9 C10 1.368(6) . ?
C10 C11 1.420(5) . ?
C11 C12 1.407(6) . ?
C11 N2 1.422(5) . ?
C12 C20 1.420(6) . ?
C12 C13 1.477(5) . ?
C13 C18 1.398(6) . ?
C13 C14 1.402(6) . ?
C14 C15 1.380(6) . ?
C15 C16 1.387(6) . ?
C16 C17 1.391(6) . ?
C16 C19 1.511(6) . ?
C17 C18 1.397(6) . ?
C20 N3 1.380(5) . ?
C20 C21 1.397(6) . ?
C21 C22 1.383(6) . ?
C22 C23 1.399(6) . ?
C23 N3 1.349(5) . ?
C23 C24 1.520(6) . ?
C24 C27 1.519(6) . ?
C24 C26 1.534(6) . ?
C24 C25 1.535(6) . ?
C27 N4 1.349(5) . ?
C27 C28 1.404(6) . ?
C28 C29 1.387(6) . ?
C29 C30 1.414(6) . ?
C30 N4 1.389(5) . ?
C30 C31 1.404(6) . ?
C31 C32 1.482(5) . ?
C32 C33 1.401(6) . ?
C32 C37 1.408(6) . ?
C33 C34 1.385(6) . ?
C34 C35 1.386(7) . ?
C35 C36 1.392(6) . ?
C35 C38 1.506(6) . ?
C36 C37 1.382(6) . ?
N1 B1 1.580(6) . ?
N2 B1 1.586(5) . ?
B1 F2 1.361(5) . ?
B1 F1 1.397(5) . ?
B2 F6A 1.265(10) . ?
B2 F6 1.316(7) . ?
B2 F5A 1.322(9) . ?
B2 F4 1.345(6) . ?
B2 F4A 1.359(9) . ?
B2 F5 1.379(7) . ?
B2 F3 1.442(7) . ?
Cl1 C39 1.743(6) . ?
Cl2 C39 1.756(6) . ?
Cl3 C39 1.749(6) . ?
Cl4 C40 1.743(8) . ?
Cl5 C40 1.686(8) . ?
C40 Cl4 1.823(13) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C31 C1 C2 121.6(4) . . ?
C31 C1 N1 130.5(4) . . ?
C2 C1 N1 107.4(3) . . ?
C3 C2 C1 108.6(4) . . ?
C2 C3 C4 106.9(4) . . ?
N1 C4 C3 110.5(3) . . ?
N1 C4 C5 122.7(4) . . ?
C3 C4 C5 126.7(4) . . ?
C8 C5 C4 112.3(3) . . ?
C8 C5 C7 109.3(3) . . ?
C4 C5 C7 109.1(4) . . ?
C8 C5 C6 108.2(4) . . ?
C4 C5 C6 109.0(3) . . ?
C7 C5 C6 108.8(4) . . ?
N2 C8 C9 111.1(4) . . ?
N2 C8 C5 123.2(3) . . ?
C9 C8 C5 125.5(4) . . ?
C10 C9 C8 106.5(4) . . ?
C9 C10 C11 108.8(4) . . ?
C12 C11 C10 121.7(4) . . ?
C12 C11 N2 131.0(4) . . ?
C10 C11 N2 107.0(3) . . ?
C11 C12 C20 127.0(4) . . ?
C11 C12 C13 115.3(4) . . ?
C20 C12 C13 117.6(4) . . ?
C18 C13 C14 117.6(4) . . ?
C18 C13 C12 123.0(4) . . ?
C14 C13 C12 119.4(4) . . ?
C15 C14 C13 121.3(4) . . ?
C14 C15 C16 120.9(4) . . ?
C15 C16 C17 118.7(4) . . ?
C15 C16 C19 119.7(4) . . ?
C17 C16 C19 121.7(4) . . ?
C16 C17 C18 120.7(4) . . ?
C17 C18 C13 120.8(4) . . ?
N3 C20 C21 106.4(3) . . ?
N3 C20 C12 124.3(4) . . ?
C21 C20 C12 129.3(4) . . ?
C22 C21 C20 108.0(4) . . ?
C21 C22 C23 107.8(4) . . ?
N3 C23 C22 107.4(4) . . ?
N3 C23 C24 123.5(4) . . ?
C22 C23 C24 129.1(4) . . ?
C27 C24 C23 105.4(3) . . ?
C27 C24 C26 111.9(3) . . ?
C23 C24 C26 111.6(3) . . ?
C27 C24 C25 108.8(3) . . ?
C23 C24 C25 109.0(3) . . ?
C26 C24 C25 110.0(4) . . ?
N4 C27 C28 107.9(4) . . ?
N4 C27 C24 123.1(3) . . ?
C28 C27 C24 128.8(4) . . ?
C29 C28 C27 107.5(4) . . ?
C28 C29 C30 108.2(4) . . ?
N4 C30 C31 124.7(4) . . ?
N4 C30 C29 105.8(4) . . ?
C31 C30 C29 129.5(4) . . ?
C30 C31 C1 127.7(4) . . ?
C30 C31 C32 116.8(4) . . ?
C1 C31 C32 115.5(4) . . ?
C33 C32 C37 117.5(4) . . ?
C33 C32 C31 122.2(4) . . ?
C37 C32 C31 120.4(4) . . ?
C34 C33 C32 120.7(4) . . ?
C33 C34 C35 122.0(4) . . ?
C34 C35 C36 117.5(4) . . ?
C34 C35 C38 121.5(4) . . ?
C36 C35 C38 121.0(4) . . ?
C37 C36 C35 121.6(4) . . ?
C36 C37 C32 120.8(4) . . ?
C4 N1 C1 106.6(3) . . ?
C4 N1 B1 116.9(3) . . ?
C1 N1 B1 131.2(3) . . ?
C8 N2 C11 106.5(3) . . ?
C8 N2 B1 116.7(3) . . ?
C11 N2 B1 131.4(3) . . ?
C23 N3 C20 110.4(3) . . ?
C27 N4 C30 110.6(3) . . ?
F2 B1 F1 109.9(3) . . ?
F2 B1 N1 113.6(3) . . ?
F1 B1 N1 107.6(3) . . ?
F2 B1 N2 113.3(3) . . ?
F1 B1 N2 106.8(3) . . ?
N1 B1 N2 105.2(3) . . ?
F6A B2 F5A 111.6(9) . . ?
F6 B2 F4 113.5(6) . . ?
F6A B2 F4A 115.6(9) . . ?
F5A B2 F4A 109.6(8) . . ?
F6 B2 F5 114.8(7) . . ?
F4 B2 F5 107.8(5) . . ?
F6A B2 F3 113.3(9) . . ?
F6 B2 F3 105.6(5) . . ?
F5A B2 F3 104.4(6) . . ?
F4 B2 F3 108.6(4) . . ?
F4A B2 F3 101.5(6) . . ?
F5 B2 F3 106.0(5) . . ?
Cl1 C39 Cl3 112.2(4) . . ?
Cl1 C39 Cl2 110.4(3) . . ?
Cl3 C39 Cl2 110.7(3) . . ?
Cl5 C40 Cl4 111.4(5) . . ?
Cl5 C40 Cl4 107.6(6) . 2_665 ?
Cl4 C40 Cl4 105.4(6) . 2_665 ?

_refine_diff_density_max         1.005
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.092

####################################################################### 
# 
# 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 1587635'
_audit_update_record             
;
2017-11-26 deposited with the CCDC.
2018-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H35 B F2 N4'
_chemical_formula_weight         596.51

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.9721(11)
_cell_length_b                   14.8594(13)
_cell_length_c                   17.2769(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3073.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    99(2)
_cell_measurement_reflns_used    36247
_cell_measurement_theta_min      1.808
_cell_measurement_theta_max      27.959

_exptl_crystal_description       Block
_exptl_crystal_colour            Black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.084
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5774
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36247
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.808
_diffrn_reflns_theta_max         27.959
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7300
_reflns_number_gt                3605
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.999

_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       'SMART (Siemens, 1995)'
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'

_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_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)+(0.0623P)²+0.4399P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1190 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.9(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7300
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1582
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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 0.0134(4) 0.0362(3) 0.0099(3) 0.0515(13) Uani 1 1 d . . . . .
C2 C -0.0070(4) -0.0183(3) -0.0550(3) 0.0491(13) Uani 1 1 d . . . . .
C3 C 0.0652(4) -0.0067(3) -0.1235(3) 0.0516(13) Uani 1 1 d . . . . .
C4 C 0.1808(4) -0.0168(4) -0.1183(3) 0.0601(14) Uani 1 1 d . . . . .
H4 H 0.212605 -0.034006 -0.071415 0.072 Uiso 1 1 calc R U . . .
C5 C 0.2487(5) -0.0017(4) -0.1815(4) 0.0644(16) Uani 1 1 d . . . . .
H5 H 0.325344 -0.010071 -0.176502 0.077 Uiso 1 1 calc R U . . .
C6 C 0.2061(5) 0.0257(4) -0.2519(3) 0.0577(14) Uani 1 1 d . . . . .
C7 C 0.2812(5) 0.0463(4) -0.3201(3) 0.0755(18) Uani 1 1 d . . . . .
H7A H 0.353775 0.063583 -0.301622 0.113 Uiso 1 1 calc R U . . .
H7B H 0.249688 0.094702 -0.349734 0.113 Uiso 1 1 calc R U . . .
H7C H 0.287911 -0.006165 -0.352137 0.113 Uiso 1 1 calc R U . . .
C8 C 0.0900(5) 0.0360(3) -0.2578(3) 0.0589(15) Uani 1 1 d . . . . .
H8 H 0.058529 0.054331 -0.304406 0.071 Uiso 1 1 calc R U . . .
C9 C 0.0219(5) 0.0191(4) -0.1947(3) 0.0597(15) Uani 1 1 d . . . . .
H9 H -0.055021 0.025242 -0.200150 0.072 Uiso 1 1 calc R U . . .
C10 C -0.0973(4) -0.0775(3) -0.0577(3) 0.0460(12) Uani 1 1 d . . . . .
C11 C -0.1344(5) -0.1322(4) -0.1187(3) 0.0547(14) Uani 1 1 d . . . . .
H11 H -0.100575 -0.139382 -0.166729 0.066 Uiso 1 1 calc R U . . .
C12 C -0.2312(5) -0.1732(4) -0.0931(3) 0.0629(16) Uani 1 1 d . . . . .
H12 H -0.275049 -0.212732 -0.121739 0.076 Uiso 1 1 calc R U . . .
C13 C -0.2527(4) -0.1453(3) -0.0169(3) 0.0520(14) Uani 1 1 d . . . . .
C14 C -0.3571(5) -0.1700(4) 0.0285(3) 0.0577(15) Uani 1 1 d . . . . .
C15 C -0.4237(5) -0.2412(4) -0.0163(3) 0.0659(16) Uani 1 1 d . . . . .
H15A H -0.441046 -0.218747 -0.066976 0.099 Uiso 1 1 calc R U . . .
H15B H -0.491660 -0.254321 0.010916 0.099 Uiso 1 1 calc R U . . .
H15C H -0.379915 -0.295082 -0.020840 0.099 Uiso 1 1 calc R U . . .
C16 C -0.3334(6) -0.2149(4) 0.1088(3) 0.089(2) Uani 1 1 d . . . . .
H16A H -0.272048 -0.256080 0.103916 0.134 Uiso 1 1 calc R U . . .
H16B H -0.398657 -0.246893 0.125679 0.134 Uiso 1 1 calc R U . . .
H16C H -0.315003 -0.169228 0.145958 0.134 Uiso 1 1 calc R U . . .
C17 C -0.4295(5) -0.0866(4) 0.0389(3) 0.0530(14) Uani 1 1 d . . . . .
C18 C -0.5388(5) -0.0735(4) 0.0117(3) 0.0669(16) Uani 1 1 d . . . . .
H18 H -0.580996 -0.114612 -0.016418 0.080 Uiso 1 1 calc R U . . .
C19 C -0.5721(5) 0.0111(4) 0.0342(3) 0.0577(14) Uani 1 1 d . . . . .
H19 H -0.641116 0.037727 0.024854 0.069 Uiso 1 1 calc R U . . .
C20 C -0.4803(4) 0.0500(4) 0.0745(3) 0.0501(13) Uani 1 1 d . . . . .
C21 C -0.4704(4) 0.1340(4) 0.1089(3) 0.0464(12) Uani 1 1 d . . . . .
C22 C -0.5663(4) 0.1988(3) 0.1051(3) 0.0463(12) Uani 1 1 d . . . . .
C23 C -0.6099(4) 0.2276(4) 0.0346(3) 0.0524(14) Uani 1 1 d . . . . .
H23 H -0.582288 0.203420 -0.011220 0.063 Uiso 1 1 calc R U . . .
C24 C -0.6931(4) 0.2912(4) 0.0317(3) 0.0533(14) Uani 1 1 d . . . . .
H24 H -0.719981 0.310453 -0.016070 0.064 Uiso 1 1 calc R U . . .
C25 C -0.7374(4) 0.3269(3) 0.0988(3) 0.0484(13) Uani 1 1 d . . . . .
C26 C -0.8297(5) 0.3967(4) 0.0964(4) 0.0708(17) Uani 1 1 d . . . . .
H26A H -0.797449 0.455589 0.091646 0.106 Uiso 1 1 calc R U . . .
H26B H -0.872699 0.393441 0.143194 0.106 Uiso 1 1 calc R U . . .
H26C H -0.877306 0.385237 0.052787 0.106 Uiso 1 1 calc R U . . .
C27 C -0.6967(4) 0.2961(4) 0.1689(3) 0.0542(14) Uani 1 1 d . . . . .
H27 H -0.727018 0.318274 0.214584 0.065 Uiso 1 1 calc R U . . .
C28 C -0.6118(5) 0.2331(4) 0.1724(3) 0.0546(14) Uani 1 1 d . . . . .
H28 H -0.585399 0.213790 0.220249 0.066 Uiso 1 1 calc R U . . .
C29 C -0.3719(4) 0.1653(3) 0.1452(3) 0.0451(12) Uani 1 1 d . . . . .
C30 C -0.3450(5) 0.2521(4) 0.1697(3) 0.0549(14) Uani 1 1 d . . . . .
H30 H -0.391866 0.301965 0.170046 0.066 Uiso 1 1 calc R U . . .
C31 C -0.2341(4) 0.2492(4) 0.1936(3) 0.0525(13) Uani 1 1 d . . . . .
H31 H -0.193507 0.297596 0.212901 0.063 Uiso 1 1 calc R U . . .
C32 C -0.1941(4) 0.1625(3) 0.1841(3) 0.0443(12) Uani 1 1 d . . . . .
C33 C -0.0788(4) 0.1262(4) 0.2010(3) 0.0518(13) Uani 1 1 d . . . . .
C34 C -0.0830(5) 0.0497(4) 0.2601(3) 0.0664(16) Uani 1 1 d . . . . .
H34A H -0.107432 0.072852 0.309173 0.100 Uiso 1 1 calc R U . . .
H34B H -0.009965 0.023848 0.265638 0.100 Uiso 1 1 calc R U . . .
H34C H -0.134334 0.004356 0.242725 0.100 Uiso 1 1 calc R U . . .
C35 C -0.0092(4) 0.2034(4) 0.2369(3) 0.0622(15) Uani 1 1 d . . . . .
H35A H -0.005508 0.252787 0.201190 0.093 Uiso 1 1 calc R U . . .
H35B H 0.064941 0.182237 0.247756 0.093 Uiso 1 1 calc R U . . .
H35C H -0.043835 0.223035 0.284095 0.093 Uiso 1 1 calc R U . . .
C36 C -0.0230(4) 0.0994(3) 0.1240(3) 0.0510(13) Uani 1 1 d . . . . .
C37 C 0.0635(5) 0.1471(4) 0.0889(3) 0.0562(14) Uani 1 1 d . . . . .
H37 H 0.099519 0.196824 0.109869 0.067 Uiso 1 1 calc R U . . .
C38 C 0.0872(4) 0.1087(3) 0.0179(3) 0.0535(13) Uani 1 1 d . . . . .
H38 H 0.141102 0.127336 -0.017338 0.064 Uiso 1 1 calc R U . . .
N1 N -0.0538(3) 0.0299(3) 0.0772(2) 0.0511(11) Uani 1 1 d . . . . .
N2 N -0.1697(3) -0.0883(3) 0.0063(2) 0.0526(11) Uani 1 1 d . . . . .
N3 N -0.3932(3) -0.0133(3) 0.0772(2) 0.0540(11) Uani 1 1 d . . . . .
N4 N -0.2781(3) 0.1116(3) 0.1554(2) 0.0450(10) Uani 1 1 d . . . . .
H4A H -0.274054 0.055098 0.145103 0.054 Uiso 1 1 calc R U . A 2
F1 F -0.0429(3) -0.1290(2) 0.11233(18) 0.0504(13) Uani 0.765(7) 1 d . . P B 1
B B -0.1202(6) -0.0635(5) 0.0915(4) 0.0428(19) Uani 0.765(7) 1 d . . P B 1
F2 F -0.1932(9) -0.0590(8) 0.1471(8) 0.052(3) Uani 0.765(7) 1 d . . P B 1
F1A F -0.3358(11) -0.0280(9) 0.2205(8) 0.068(5) Uiso 0.235(7) 1 d . . P B 2
B1A B -0.293(2) -0.0037(18) 0.1528(14) 0.049(7) Uiso 0.235(7) 1 d . . P B 2
F2A F -0.212(3) -0.051(2) 0.146(2) 0.023(6) Uiso 0.235(7) 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C38 1.401(7) . ?
C1 C2 1.405(7) . ?
C1 N1 1.416(6) . ?
C2 C10 1.394(7) . ?
C2 C3 1.476(7) . ?
C3 C9 1.389(7) . ?
C3 C4 1.395(7) . ?
C4 C5 1.380(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(8) . ?
C5 H5 0.9300 . ?
C6 C8 1.402(7) . ?
C6 C7 1.513(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.384(7) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.403(7) . ?
C10 N2 1.414(6) . ?
C11 C12 1.382(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.404(7) . ?
C12 H12 0.9300 . ?
C13 N2 1.366(6) . ?
C13 C14 1.521(8) . ?
C14 C17 1.523(8) . ?
C14 C15 1.534(7) . ?
C14 C16 1.564(7) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N3 1.347(6) . ?
C17 C18 1.404(8) . ?
C18 C19 1.375(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.424(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.389(7) . ?
C20 N3 1.404(6) . ?
C21 C29 1.414(7) . ?
C21 C22 1.500(7) . ?
C22 C28 1.382(7) . ?
C22 C23 1.393(6) . ?
C23 C24 1.374(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.381(7) . ?
C24 H24 0.9300 . ?
C25 C27 1.382(7) . ?
C25 C26 1.516(7) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.382(7) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 N4 1.388(6) . ?
C29 C30 1.396(7) . ?
C30 C31 1.390(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.384(7) . ?
C31 H31 0.9300 . ?
C32 N4 1.352(6) . ?
C32 C33 1.511(7) . ?
C33 C34 1.530(7) . ?
C33 C36 1.541(7) . ?
C33 C35 1.548(7) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 N1 1.363(6) . ?
C36 C37 1.393(7) . ?
C37 C38 1.381(7) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
N1 B 1.619(9) . ?
N2 B 1.628(8) . ?
N3 B1A 1.78(3) . ?
N4 B1A 1.72(3) . ?
N4 H4A 0.8600 . ?
F1A B1A 1.33(3) . ?
B1A F2A 1.21(4) . ?

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
C38 C1 C2 129.2(5) . . ?
C38 C1 N1 109.1(4) . . ?
C2 C1 N1 121.2(4) . . ?
C10 C2 C1 121.6(5) . . ?
C10 C2 C3 120.1(5) . . ?
C1 C2 C3 118.1(5) . . ?
C9 C3 C4 117.3(5) . . ?
C9 C3 C2 121.6(5) . . ?
C4 C3 C2 121.1(5) . . ?
C5 C4 C3 121.0(6) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 121.9(5) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C8 117.5(5) . . ?
C5 C6 C7 121.7(5) . . ?
C8 C6 C7 120.7(5) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C6 120.5(5) . . ?
C9 C8 H8 119.8 . . ?
C6 C8 H8 119.8 . . ?
C8 C9 C3 121.8(5) . . ?
C8 C9 H9 119.1 . . ?
C3 C9 H9 119.1 . . ?
C2 C10 C11 129.4(5) . . ?
C2 C10 N2 121.4(4) . . ?
C11 C10 N2 109.1(5) . . ?
C12 C11 C10 106.3(5) . . ?
C12 C11 H11 126.8 . . ?
C10 C11 H11 126.8 . . ?
C11 C12 C13 108.8(5) . . ?
C11 C12 H12 125.6 . . ?
C13 C12 H12 125.6 . . ?
N2 C13 C12 109.0(5) . . ?
N2 C13 C14 126.6(5) . . ?
C12 C13 C14 124.3(5) . . ?
C13 C14 C17 109.4(4) . . ?
C13 C14 C15 109.4(4) . . ?
C17 C14 C15 109.0(5) . . ?
C13 C14 C16 114.2(5) . . ?
C17 C14 C16 110.2(5) . . ?
C15 C14 C16 104.3(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 110.7(5) . . ?
N3 C17 C14 122.2(5) . . ?
C18 C17 C14 127.1(5) . . ?
C19 C18 C17 107.6(5) . . ?
C19 C18 H18 126.2 . . ?
C17 C18 H18 126.2 . . ?
C18 C19 C20 106.5(5) . . ?
C18 C19 H19 126.7 . . ?
C20 C19 H19 126.7 . . ?
C21 C20 N3 121.6(4) . . ?
C21 C20 C19 129.8(5) . . ?
N3 C20 C19 108.6(5) . . ?
C20 C21 C29 123.8(5) . . ?
C20 C21 C22 119.6(4) . . ?
C29 C21 C22 116.6(4) . . ?
C28 C22 C23 118.3(5) . . ?
C28 C22 C21 120.2(4) . . ?
C23 C22 C21 121.5(4) . . ?
C24 C23 C22 121.0(5) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 120.7(5) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C24 C25 C27 118.3(5) . . ?
C24 C25 C26 121.2(5) . . ?
C27 C25 C26 120.5(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 C28 121.5(5) . . ?
C25 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C22 C28 C27 120.1(4) . . ?
C22 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
N4 C29 C30 107.8(4) . . ?
N4 C29 C21 122.9(4) . . ?
C30 C29 C21 129.1(5) . . ?
C31 C30 C29 106.4(5) . . ?
C31 C30 H30 126.8 . . ?
C29 C30 H30 126.8 . . ?
C32 C31 C30 108.9(5) . . ?
C32 C31 H31 125.5 . . ?
C30 C31 H31 125.5 . . ?
N4 C32 C31 107.8(4) . . ?
N4 C32 C33 123.4(4) . . ?
C31 C32 C33 128.7(5) . . ?
C32 C33 C34 111.4(4) . . ?
C32 C33 C36 108.8(4) . . ?
C34 C33 C36 113.5(4) . . ?
C32 C33 C35 107.7(4) . . ?
C34 C33 C35 107.5(4) . . ?
C36 C33 C35 107.7(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N1 C36 C37 109.2(5) . . ?
N1 C36 C33 126.2(5) . . ?
C37 C36 C33 124.6(5) . . ?
C38 C37 C36 109.2(5) . . ?
C38 C37 H37 125.4 . . ?
C36 C37 H37 125.4 . . ?
C37 C38 C1 106.0(5) . . ?
C37 C38 H38 127.0 . . ?
C1 C38 H38 127.0 . . ?
C36 N1 C1 106.4(4) . . ?
C36 N1 B 133.8(4) . . ?
C1 N1 B 117.4(4) . . ?
C13 N2 C10 106.7(4) . . ?
C13 N2 B 132.0(5) . . ?
C10 N2 B 117.3(4) . . ?
C17 N3 C20 106.6(4) . . ?
C17 N3 B1A 130.0(10) . . ?
C20 N3 B1A 118.2(9) . . ?
C32 N4 C29 109.1(4) . . ?
C32 N4 B1A 130.0(10) . . ?
C29 N4 B1A 119.0(10) . . ?
C32 N4 H4A 125.5 . . ?
C29 N4 H4A 125.5 . . ?
B1A N4 H4A 13.9 . . ?


_refine_diff_density_max         0.236
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.056


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dichloromethane/n-hexane'
####################################################################### 
# 
# 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_Compound_6b
_database_code_depnum_ccdc_archive 'CCDC 1587637'
_audit_update_record             
;
2018-01-14 deposited with the CCDC.
2018-01-31 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         'C36 H20 B2 F12 N4 O'
_chemical_formula_sum            'C36 H20 B2 F12 N4 O'
_chemical_formula_weight         774.18

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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                   16.1693(10)
_cell_length_b                   17.8717(11)
_cell_length_c                   18.1564(11)
_cell_angle_alpha                83.225(4)
_cell_angle_beta                 79.773(4)
_cell_angle_gamma                67.472(4)
_cell_volume                     4762.1(5)
_cell_formula_units_Z            6
_cell_measurement_temperature    99(2)
_cell_measurement_reflns_used    151819
_cell_measurement_theta_min      1.141
_cell_measurement_theta_max      27.928

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_F_000             2340
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.147
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2009
_exptl_absorpt_correction_T_max  0.2621
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'Area detector ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            151819
_diffrn_reflns_av_unetI/netI     0.1850
_diffrn_reflns_av_R_equivalents  0.1883
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.141
_diffrn_reflns_theta_max         27.928
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             22188
_reflns_number_gt                4573
_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       'SMART (Siemens, 1995)'
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_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)+(0.0848P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         22188
_refine_ls_number_parameters     1475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3002
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2546
_refine_ls_wR_factor_gt          0.1676
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.943
_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
B1A B 0.2801(12) 0.3298(12) 0.3433(11) 0.016(5) Uiso 0.486(9) 1 d . . P A 1
F2A F 0.4319(6) 0.3882(6) 0.1987(5) 0.032(3) Uiso 0.486(9) 1 d . . P A 1
O1E O 0.3203(10) 0.3509(10) 0.2757(9) 0.022(4) Uiso 0.486(9) 1 d . . P A 1
B2A B 0.4035(14) 0.3621(14) 0.2680(13) 0.029(6) Uiso 0.486(9) 1 d . . P A 1
F1F F 0.3352(10) 0.3077(10) 0.4012(9) 0.021(4) Uiso 0.486(9) 1 d . . P A 1
B1B B 0.2624(14) 0.3127(14) 0.3955(13) 0.033(6) Uiso 0.514(9) 1 d . . P A 2
F1B F 0.2381(7) 0.2756(7) 0.4666(6) 0.046(4) Uiso 0.514(9) 1 d . . P A 2
O1F O 0.3464(14) 0.3113(13) 0.3886(11) 0.039(7) Uiso 0.514(9) 1 d . . P A 2
B2B B 0.3866(16) 0.3388(16) 0.3242(14) 0.040(6) Uiso 0.514(9) 1 d . . P A 2
F1E F 0.3302(9) 0.3642(8) 0.2634(7) 0.028(4) Uiso 0.514(9) 1 d . . P A 2
B20A B 0.2972(10) 0.9142(10) 0.2700(9) 0.014(4) Uiso 0.498(9) 1 d . . P B 1
F11A F 0.3069(6) 0.9743(6) 0.2245(5) 0.027(3) Uiso 0.498(9) 1 d . . P B 1
O14A O 0.3802(9) 0.8647(10) 0.2925(8) 0.031(4) Uiso 0.498(9) 1 d . . P B 1
B10A B 0.3836(12) 0.7945(12) 0.3495(10) 0.016(4) Uiso 0.498(9) 1 d . . P B 1
F14B F 0.2945(8) 0.8006(8) 0.3615(7) 0.032(4) Uiso 0.498(9) 1 d . . P B 1
B20B B 0.2821(16) 0.8726(16) 0.3192(14) 0.041(7) Uiso 0.502(9) 1 d . . P B 2
O14B O 0.3032(10) 0.7784(10) 0.3780(8) 0.028(4) Uiso 0.502(9) 1 d . . P B 2
F14A F 0.3579(7) 0.8883(7) 0.2995(6) 0.025(3) Uiso 0.502(9) 1 d . . P B 2
F10B F 0.3617(6) 0.6917(6) 0.4378(5) 0.029(3) Uiso 0.502(9) 1 d . . P B 2
B10B B 0.3706(13) 0.7577(12) 0.3857(11) 0.021(5) Uiso 0.502(9) 1 d . . P B 2
B30A B 0.9436(13) 0.5385(13) 0.9855(12) 0.025(5) Uiso 0.5 1 d . . P C 1
F32A F 1.0422(7) 0.5317(7) 0.9682(6) 0.020(3) Uiso 0.5 1 d . . P C 1
O32A O 1.0269(8) 0.5595(8) 0.9573(7) 0.017(3) Uiso 0.5 1 d . . P C 2
B30B B 0.9578(16) 0.5784(16) 0.9480(14) 0.041(6) Uiso 0.5 1 d . . P C 2
F31B F 0.9725(6) 0.6404(6) 0.8916(5) 0.030(3) Uiso 0.5 1 d . . P C 2
B31B B 0.0525(12) 0.0040(12) 0.9886(11) 0.019(4) Uiso 0.5 1 d . . P D 1
F32B F 0.0007(9) 0.0273(8) 0.9295(7) 0.026(4) Uiso 0.5 1 d . . P D 1
O31D O -0.0164(9) 0.0249(8) 0.9420(8) 0.012(4) Uiso 0.5 1 d . . P D 1
B31C B 0.0683(14) 0.0270(14) 0.9375(13) 0.030(5) Uiso 0.5 1 d . . P D 2
F30A F 0.0978(6) 0.0528(6) 0.8659(5) 0.033(3) Uiso 0.5 1 d . . P D 2
C1 C 0.3246(5) 0.1824(5) 0.2997(5) 0.028(2) Uani 1 1 d . . . . .
C2 C 0.2733(7) 0.1371(6) 0.2897(5) 0.039(3) Uani 1 1 d . . . . .
H2 H 0.2971 0.0853 0.2719 0.047 Uiso 1 1 calc R U . . .
C3 C 0.1843(6) 0.1800(7) 0.3097(5) 0.045(3) Uani 1 1 d . . . . .
H3 H 0.1369 0.1639 0.3060 0.054 Uiso 1 1 calc R U . . .
C4 C 0.1763(6) 0.2523(6) 0.3367(5) 0.025(2) Uani 1 1 d . . . . .
C5 C 0.0895(6) 0.3197(6) 0.3685(6) 0.035(3) Uani 1 1 d . . . . .
C6 C 0.0238(6) 0.3419(6) 0.3107(6) 0.053(3) Uani 1 1 d . . . . .
H6A H 0.0128 0.2947 0.3022 0.080 Uiso 1 1 calc R U . . .
H6B H -0.0323 0.3834 0.3294 0.080 Uiso 1 1 calc R U . . .
H6C H 0.0498 0.3614 0.2645 0.080 Uiso 1 1 calc R U . . .
C7 C 0.0530(7) 0.2848(7) 0.4439(6) 0.058(4) Uani 1 1 d . . . . .
H7A H 0.0425 0.2374 0.4353 0.087 Uiso 1 1 calc R U . . .
H7B H 0.0966 0.2705 0.4779 0.087 Uiso 1 1 calc R U . . .
H7C H -0.0027 0.3248 0.4653 0.087 Uiso 1 1 calc R U . . .
C8 C 0.1061(6) 0.3937(6) 0.3812(6) 0.035(3) Uani 1 1 d . . . . .
C9 C 0.0410(6) 0.4688(6) 0.4003(6) 0.042(3) Uani 1 1 d . . . . .
H9 H -0.0215 0.4835 0.4073 0.051 Uiso 1 1 calc R U . . .
C10 C 0.0886(6) 0.5178(6) 0.4068(6) 0.042(3) Uani 1 1 d . . . . .
H10 H 0.0628 0.5714 0.4203 0.050 Uiso 1 1 calc R U . . .
C11 C 0.1824(6) 0.4728(6) 0.3898(5) 0.031(2) Uani 1 1 d . . . . .
C12 C 0.2495(6) 0.5077(6) 0.3858(5) 0.026(2) Uani 1 1 d . . . . .
C13 C 0.2087(6) 0.5947(6) 0.4143(6) 0.031(2) Uani 1 1 d . . . . .
C14 C 0.2068(6) 0.6081(7) 0.4886(6) 0.036(3) Uani 1 1 d . . . . .
C15 C 0.1756(6) 0.6841(7) 0.5105(6) 0.037(3) Uani 1 1 d . . . . .
C16 C 0.1396(6) 0.7504(7) 0.4649(6) 0.036(3) Uani 1 1 d . . . . .
C17 C 0.1389(6) 0.7381(6) 0.3925(7) 0.046(3) Uani 1 1 d . . . . .
C18 C 0.1729(6) 0.6587(6) 0.3665(6) 0.032(2) Uani 1 1 d . . . . .
C19 C 0.3449(6) 0.4826(6) 0.3655(5) 0.030(2) Uani 1 1 d . . . . .
C20 C 0.3926(5) 0.5322(6) 0.3778(5) 0.031(2) Uani 1 1 d . . . . .
H20 H 0.3675 0.5834 0.3971 0.037 Uiso 1 1 calc R U . . .
C21 C 0.4838(6) 0.4885(6) 0.3549(6) 0.041(3) Uani 1 1 d . . . . .
H21 H 0.5315 0.5048 0.3566 0.049 Uiso 1 1 calc R U . . .
C22 C 0.4905(5) 0.4152(6) 0.3290(5) 0.031(3) Uani 1 1 d . . . . .
C23 C 0.5758(5) 0.3475(6) 0.2967(5) 0.027(2) Uani 1 1 d . . . . .
C24 C 0.6460(6) 0.3242(7) 0.3516(6) 0.051(3) Uani 1 1 d . . . . .
H24A H 0.6574 0.3713 0.3596 0.077 Uiso 1 1 calc R U . . .
H24B H 0.6227 0.3036 0.3986 0.077 Uiso 1 1 calc R U . . .
H24C H 0.7013 0.2833 0.3308 0.077 Uiso 1 1 calc R U . . .
C25 C 0.6122(7) 0.3805(6) 0.2215(6) 0.054(3) Uani 1 1 d . . . . .
H25A H 0.6229 0.4281 0.2291 0.080 Uiso 1 1 calc R U . . .
H25B H 0.6678 0.3399 0.2007 0.080 Uiso 1 1 calc R U . . .
H25C H 0.5686 0.3941 0.1876 0.080 Uiso 1 1 calc R U . . .
C26 C 0.5591(6) 0.2737(6) 0.2852(5) 0.030(2) Uani 1 1 d . . . . .
C27 C 0.6232(7) 0.1957(7) 0.2649(6) 0.045(3) Uani 1 1 d . . . . .
H27 H 0.6857 0.1812 0.2567 0.054 Uiso 1 1 calc R U . . .
C28 C 0.5804(6) 0.1467(6) 0.2597(5) 0.037(3) Uani 1 1 d . . . . .
H28 H 0.6075 0.0926 0.2477 0.044 Uiso 1 1 calc R U . . .
C29 C 0.4831(5) 0.1925(6) 0.2760(5) 0.027(2) Uani 1 1 d . . . . .
C30 C 0.4187(6) 0.1597(6) 0.2792(5) 0.031(2) Uani 1 1 d . . . . .
C31 C 0.4584(5) 0.0747(6) 0.2535(6) 0.030(3) Uani 1 1 d . . . . .
C32 C 0.4587(6) 0.0606(6) 0.1803(6) 0.036(3) Uani 1 1 d . . . . .
C33 C 0.4953(6) -0.0184(6) 0.1527(6) 0.031(3) Uani 1 1 d . . . . .
C34 C 0.5264(6) -0.0813(6) 0.2046(6) 0.037(3) Uani 1 1 d . . . . .
C35 C 0.5279(6) -0.0689(6) 0.2770(5) 0.030(2) Uani 1 1 d . . . . .
C36 C 0.4929(5) 0.0073(6) 0.2998(6) 0.037(3) Uani 1 1 d . . . . .
N1 N 0.1898(4) 0.3954(5) 0.3755(4) 0.030(2) Uani 1 1 d . . . . .
N2 N 0.4071(5) 0.4127(5) 0.3346(4) 0.032(2) Uani 1 1 d . . . . .
N3 N 0.4770(5) 0.2711(5) 0.2914(4) 0.030(2) Uani 1 1 d . . . . .
N4 N 0.2578(4) 0.2551(5) 0.3328(4) 0.0266(19) Uani 1 1 d . . . . .
F1 F 0.1713(3) 0.6492(4) 0.2943(3) 0.0414(16) Uani 1 1 d . . . . .
F2 F 0.1043(4) 0.8000(4) 0.3422(4) 0.0548(18) Uani 1 1 d . . . . .
F3 F 0.1067(4) 0.8251(4) 0.4861(4) 0.0570(19) Uani 1 1 d . . . . .
F4 F 0.1746(4) 0.6961(4) 0.5838(3) 0.0537(18) Uani 1 1 d . . . . .
F5 F 0.2395(4) 0.5445(4) 0.5373(3) 0.0513(17) Uani 1 1 d . . . . .
F6 F 0.4275(4) 0.1220(4) 0.1295(3) 0.0443(16) Uani 1 1 d . . . . .
F7 F 0.4940(4) -0.0308(4) 0.0823(3) 0.0490(17) Uani 1 1 d . . . . .
F8 F 0.5609(4) -0.1596(3) 0.1793(3) 0.0506(17) Uani 1 1 d . . . . .
F9 F 0.5617(4) -0.1347(4) 0.3226(4) 0.0579(19) Uani 1 1 d . . . . .
F10 F 0.4966(4) 0.0171(4) 0.3706(3) 0.0477(17) Uani 1 1 d . . . . .
C301 C 0.3120(6) -0.0067(7) 1.0204(6) 0.055(3) Uani 1 1 d . . . . .
H30A H 0.3658 -0.0503 1.0012 0.083 Uiso 1 1 calc R U . . .
H30B H 0.3264 0.0398 1.0248 0.083 Uiso 1 1 calc R U . . .
H30C H 0.2876 -0.0234 1.0688 0.083 Uiso 1 1 calc R U . . .
C302 C 0.2400(6) 0.0158(7) 0.9653(6) 0.040(3) Uani 1 1 d . . . . .
C303 C 0.2825(8) 0.0447(7) 0.8892(6) 0.065(4) Uani 1 1 d . . . . .
H30D H 0.3362 0.0012 0.8698 0.097 Uiso 1 1 calc R U . . .
H30E H 0.2398 0.0608 0.8542 0.097 Uiso 1 1 calc R U . . .
H30F H 0.2976 0.0900 0.8965 0.097 Uiso 1 1 calc R U . . .
C304 C 0.1577(6) 0.0826(6) 0.9949(5) 0.030(2) Uani 1 1 d . . . . .
C305 C 0.1490(6) 0.1533(6) 1.0226(6) 0.043(3) Uani 1 1 d . . . . .
H305 H 0.1964 0.1695 1.0258 0.052 Uiso 1 1 calc R U . . .
C306 C 0.0599(6) 0.1963(7) 1.0448(5) 0.040(3) Uani 1 1 d . . . . .
H306 H 0.0356 0.2472 1.0647 0.047 Uiso 1 1 calc R U . . .
C307 C 0.0117(6) 0.1502(6) 1.0323(5) 0.029(2) Uani 1 1 d . . . . .
C308 C -0.0835(6) 0.1729(6) 1.0539(5) 0.031(2) Uani 1 1 d . . . . .
C309 C 0.1525(6) -0.1395(6) 0.9440(5) 0.027(2) Uani 1 1 d . . . . .
C310 C 0.2446(6) -0.1852(6) 0.9282(5) 0.030(2) Uani 1 1 d . . . . .
H310 H 0.2702 -0.2393 0.9161 0.036 Uiso 1 1 calc R U . . .
C311 C 0.2902(7) -0.1370(7) 0.9336(6) 0.049(3) Uani 1 1 d . . . . .
H311 H 0.3528 -0.1520 0.9262 0.058 Uiso 1 1 calc R U . . .
C312 C 0.2262(6) -0.0604(6) 0.9525(5) 0.026(2) Uani 1 1 d . . . . .
C313 C -0.1239(6) 0.2562(6) 1.0816(5) 0.025(2) Uani 1 1 d . . . . .
C314 C -0.1593(6) 0.3268(6) 1.0338(5) 0.035(3) Uani 1 1 d . . . . .
C315 C -0.1943(6) 0.4043(6) 1.0568(6) 0.035(3) Uani 1 1 d . . . . .
C316 C -0.1928(6) 0.4173(6) 1.1300(7) 0.042(3) Uani 1 1 d . . . . .
C317 C -0.1573(6) 0.3506(7) 1.1793(6) 0.039(3) Uani 1 1 d . . . . .
C318 C -0.1273(6) 0.2744(6) 1.1543(5) 0.029(2) Uani 1 1 d . . . . .
N301 N 0.1440(5) -0.0624(5) 0.9581(4) 0.033(2) Uani 1 1 d . . . . .
N302 N 0.0758(5) 0.0781(5) 1.0008(4) 0.0251(19) Uani 1 1 d . . . . .
F301 F -0.0955(3) 0.2115(3) 1.2046(3) 0.0450(16) Uani 1 1 d . . . . .
F302 F -0.1599(4) 0.3626(4) 1.2504(3) 0.0532(17) Uani 1 1 d . . . . .
F303 F -0.2265(4) 0.4914(3) 1.1537(3) 0.0535(18) Uani 1 1 d . . . . .
F304 F -0.2298(4) 0.4664(3) 1.0088(3) 0.0518(18) Uani 1 1 d . . . . .
F305 F -0.1617(4) 0.3154(3) 0.9614(3) 0.0497(17) Uani 1 1 d . . . . .
C101 C 0.3750(6) 0.8715(6) 0.4673(5) 0.031(2) Uani 1 1 d . . . . .
C102 C 0.4383(6) 0.8665(6) 0.5158(5) 0.035(3) Uani 1 1 d . . . . .
H102 H 0.4275 0.9019 0.5532 0.042 Uiso 1 1 calc R U . . .
C103 C 0.5157(7) 0.8027(6) 0.4988(5) 0.039(3) Uani 1 1 d . . . . .
H103 H 0.5684 0.7879 0.5200 0.047 Uiso 1 1 calc R U . . .
C104 C 0.5006(6) 0.7616(6) 0.4410(5) 0.033(3) Uani 1 1 d . . . . .
C105 C 0.5641(6) 0.6836(5) 0.4058(5) 0.029(2) Uani 1 1 d . . . . .
C106 C 0.5592(7) 0.6126(6) 0.4600(6) 0.050(3) Uani 1 1 d . . . . .
H10A H 0.4986 0.6135 0.4684 0.075 Uiso 1 1 calc R U . . .
H10B H 0.5997 0.5624 0.4388 0.075 Uiso 1 1 calc R U . . .
H10C H 0.5764 0.6172 0.5067 0.075 Uiso 1 1 calc R U . . .
C107 C 0.6598(6) 0.6799(6) 0.3942(6) 0.042(3) Uani 1 1 d . . . . .
H10D H 0.6766 0.6832 0.4415 0.062 Uiso 1 1 calc R U . . .
H10E H 0.6995 0.6297 0.3726 0.062 Uiso 1 1 calc R U . . .
H10F H 0.6645 0.7245 0.3610 0.062 Uiso 1 1 calc R U . . .
C108 C 0.5365(6) 0.6785(5) 0.3318(6) 0.033(3) Uani 1 1 d . . . . .
C109 C 0.5912(7) 0.6325(7) 0.2705(6) 0.042(3) Uani 1 1 d . . . . .
H109 H 0.6525 0.6005 0.2671 0.050 Uiso 1 1 calc R U . . .
C110 C 0.5363(6) 0.6443(6) 0.2166(6) 0.039(3) Uani 1 1 d . . . . .
H110 H 0.5538 0.6196 0.1711 0.046 Uiso 1 1 calc R U . . .
C111 C 0.4480(6) 0.7010(6) 0.2423(5) 0.029(2) Uani 1 1 d . . . . .
C112 C 0.3776(6) 0.7301(6) 0.1995(6) 0.037(3) Uani 1 1 d . . . . .
C113 C 0.3955(6) 0.6800(6) 0.1329(6) 0.037(3) Uani 1 1 d . . . . .
C114 C 0.4258(5) 0.7067(6) 0.0604(6) 0.032(3) Uani 1 1 d . . . . .
C115 C 0.4334(6) 0.6669(7) -0.0010(6) 0.033(3) Uani 1 1 d . . . . .
C116 C 0.4127(6) 0.5946(6) 0.0086(6) 0.036(3) Uani 1 1 d . . . . .
C117 C 0.3873(6) 0.5672(6) 0.0780(6) 0.033(3) Uani 1 1 d . . . . .
C118 C 0.3802(6) 0.6100(7) 0.1387(6) 0.034(3) Uani 1 1 d . . . . .
C119 C 0.2909(6) 0.7946(6) 0.1997(5) 0.030(2) Uani 1 1 d . . . . .
C120 C 0.2276(6) 0.7977(6) 0.1519(5) 0.033(3) Uani 1 1 d . . . . .
H120 H 0.2355 0.7599 0.1176 0.039 Uiso 1 1 calc R U . . .
C121 C 0.1521(5) 0.8683(6) 0.1667(5) 0.033(3) Uani 1 1 d . . . . .
H121 H 0.1014 0.8877 0.1423 0.039 Uiso 1 1 calc R U . . .
C122 C 0.1663(6) 0.9050(6) 0.2247(5) 0.028(2) Uani 1 1 d . . . . .
C123 C 0.1052(6) 0.9834(6) 0.2598(5) 0.033(3) Uani 1 1 d . . . . .
C124 C 0.1128(7) 1.0538(6) 0.2036(5) 0.043(3) Uani 1 1 d . . . . .
H12A H 0.0745 1.1048 0.2244 0.065 Uiso 1 1 calc R U . . .
H12B H 0.1744 1.0506 0.1944 0.065 Uiso 1 1 calc R U . . .
H12C H 0.0943 1.0497 0.1574 0.065 Uiso 1 1 calc R U . . .
C125 C 0.0067(5) 0.9882(6) 0.2701(5) 0.031(2) Uani 1 1 d . . . . .
H12D H -0.0328 1.0380 0.2924 0.047 Uiso 1 1 calc R U . . .
H12E H -0.0096 0.9865 0.2222 0.047 Uiso 1 1 calc R U . . .
H12F H 0.0011 0.9431 0.3021 0.047 Uiso 1 1 calc R U . . .
C126 C 0.1311(6) 0.9882(6) 0.3351(5) 0.033(3) Uani 1 1 d . . . . .
C127 C 0.0790(6) 1.0331(6) 0.3943(5) 0.035(3) Uani 1 1 d . . . . .
H127 H 0.0184 1.0671 0.3968 0.042 Uiso 1 1 calc R U . . .
C128 C 0.1313(6) 1.0191(6) 0.4481(5) 0.036(3) Uani 1 1 d . . . . .
H128 H 0.1126 1.0420 0.4946 0.043 Uiso 1 1 calc R U . . .
C129 C 0.2193(6) 0.9641(6) 0.4230(6) 0.040(3) Uani 1 1 d . . . . .
C130 C 0.2906(6) 0.9335(6) 0.4677(6) 0.035(3) Uani 1 1 d . . . . .
C131 C 0.2714(6) 0.9850(6) 0.5320(5) 0.032(2) Uani 1 1 d . . . . .
C132 C 0.2423(7) 0.9603(7) 0.6048(6) 0.045(3) Uani 1 1 d . . . . .
C133 C 0.2340(6) 1.0025(7) 0.6680(6) 0.033(3) Uani 1 1 d . . . . .
C134 C 0.2528(6) 1.0682(7) 0.6579(6) 0.041(3) Uani 1 1 d . . . . .
C135 C 0.2792(7) 1.0998(7) 0.5871(6) 0.039(3) Uani 1 1 d . . . . .
C136 C 0.2898(6) 1.0566(6) 0.5259(6) 0.036(3) Uani 1 1 d . . . . .
N101 N 0.4183(5) 0.8037(5) 0.4242(4) 0.0289(19) Uani 1 1 d . . . . .
N102 N 0.4530(5) 0.7184(4) 0.3136(5) 0.035(2) Uani 1 1 d . . . . .
N103 N 0.2492(5) 0.8630(5) 0.2424(4) 0.033(2) Uani 1 1 d . . . . .
N104 N 0.2147(5) 0.9472(5) 0.3507(4) 0.035(2) Uani 1 1 d . . . . .
F101 F 0.4444(4) 0.7741(4) 0.0515(3) 0.0531(17) Uani 1 1 d . . . . .
F102 F 0.4603(4) 0.6911(4) -0.0705(3) 0.0500(17) Uani 1 1 d . . . . .
F103 F 0.4203(4) 0.5545(4) -0.0524(3) 0.0524(18) Uani 1 1 d . . . . .
F104 F 0.3718(4) 0.4983(4) 0.0857(3) 0.0535(17) Uani 1 1 d . . . . .
F105 F 0.3526(4) 0.5817(4) 0.2069(3) 0.0519(17) Uani 1 1 d . . . . .
F106 F 0.2228(4) 0.8923(4) 0.6162(3) 0.0518(17) Uani 1 1 d . . . . .
F107 F 0.2075(4) 0.9748(4) 0.7370(3) 0.0523(18) Uani 1 1 d . . . . .
F108 F 0.2463(4) 1.1123(4) 0.7180(3) 0.0512(17) Uani 1 1 d . . . . .
F109 F 0.2952(4) 1.1685(4) 0.5793(4) 0.0585(19) Uani 1 1 d . . . . .
F110 F 0.3150(4) 1.0853(4) 0.4594(3) 0.0459(16) Uani 1 1 d . . . . .
C201 C 0.6711(6) 0.6551(6) 0.9404(6) 0.044(3) Uani 1 1 d . . . . .
H20A H 0.6541 0.6505 0.8936 0.067 Uiso 1 1 calc R U . . .
H20B H 0.6648 0.6121 0.9752 0.067 Uiso 1 1 calc R U . . .
H20C H 0.6326 0.7065 0.9603 0.067 Uiso 1 1 calc R U . . .
C202 C 0.7775(6) 0.7214(5) 0.8725(5) 0.038(3) Uani 1 1 d . . . . .
H20D H 0.7615 0.7165 0.8253 0.058 Uiso 1 1 calc R U . . .
H20E H 0.7361 0.7714 0.8934 0.058 Uiso 1 1 calc R U . . .
H20F H 0.8379 0.7211 0.8649 0.058 Uiso 1 1 calc R U . . .
C203 C 0.7724(6) 0.6487(6) 0.9275(5) 0.031(2) Uani 1 1 d . . . . .
C204 C 0.7974(6) 0.6560(6) 1.0016(5) 0.027(2) Uani 1 1 d . . . . .
C205 C 0.7428(6) 0.7017(6) 1.0629(5) 0.038(3) Uani 1 1 d . . . . .
H205 H 0.6817 0.7343 1.0663 0.045 Uiso 1 1 calc R U . . .
C206 C 0.7990(6) 0.6883(6) 1.1176(6) 0.040(3) Uani 1 1 d . . . . .
H206 H 0.7829 0.7123 1.1634 0.048 Uiso 1 1 calc R U . . .
C207 C 0.8835(6) 0.6323(6) 1.0903(6) 0.038(3) Uani 1 1 d . . . . .
C208 C 0.9583(6) 0.6025(6) 1.1352(5) 0.031(2) Uani 1 1 d . . . . .
C209 C 0.9573(6) 0.4610(6) 0.8656(6) 0.035(3) Uani 1 1 d . . . . .
C210 C 0.8932(6) 0.4668(6) 0.8196(5) 0.033(3) Uani 1 1 d . . . . .
H210 H 0.9011 0.4303 0.7840 0.040 Uiso 1 1 calc R U . . .
C211 C 0.8185(6) 0.5338(6) 0.8355(6) 0.041(3) Uani 1 1 d . . . . .
H211 H 0.7660 0.5513 0.8134 0.050 Uiso 1 1 calc R U . . .
C212 C 0.8342(6) 0.5708(5) 0.8893(5) 0.028(2) Uani 1 1 d . . . . .
C213 C 0.9367(6) 0.6518(6) 1.2021(6) 0.032(2) Uani 1 1 d . . . . .
C214 C 0.9098(6) 0.6276(7) 1.2733(6) 0.037(3) Uani 1 1 d . . . . .
C215 C 0.8992(6) 0.6691(7) 1.3341(6) 0.045(3) Uani 1 1 d . . . . .
C216 C 0.9193(6) 0.7381(6) 1.3268(6) 0.037(3) Uani 1 1 d . . . . .
C217 C 0.9452(7) 0.7648(7) 1.2553(6) 0.042(3) Uani 1 1 d . . . . .
C218 C 0.9523(6) 0.7249(6) 1.1937(6) 0.033(3) Uani 1 1 d . . . . .
N201 N 0.8824(5) 0.6141(5) 1.0180(5) 0.036(2) Uani 1 1 d . . . . .
N202 N 0.9170(5) 0.5299(5) 0.9106(4) 0.031(2) Uani 1 1 d . . . . .
F201 F 0.8917(4) 0.5587(4) 1.2831(3) 0.0516(17) Uani 1 1 d . . . . .
F202 F 0.8739(4) 0.6413(4) 1.4021(3) 0.0478(16) Uani 1 1 d . . . . .
F203 F 0.9130(4) 0.7765(4) 1.3851(3) 0.0486(16) Uani 1 1 d . . . . .
F204 F 0.9622(4) 0.8339(4) 1.2470(3) 0.0581(18) Uani 1 1 d . . . . .
F205 F 0.9819(4) 0.7515(3) 1.1248(3) 0.0444(16) 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
B1A O1E 1.37(2) . ?
B1A F1F 1.42(3) . ?
B1A N1 1.548(19) . ?
B1A N4 1.55(2) . ?
F2A B2A 1.35(2) . ?
O1E B2A 1.41(3) . ?
B2A N2 1.62(3) . ?
B2A N3 1.67(2) . ?
B1B O1F 1.33(3) . ?
B1B F1B 1.44(2) . ?
B1B N1 1.55(2) . ?
B1B N4 1.65(2) . ?
O1F B2B 1.37(3) . ?
B2B F1E 1.48(3) . ?
B2B N2 1.52(3) . ?
B2B N3 1.57(2) . ?
B20A F11A 1.318(18) . ?
B20A O14A 1.40(2) . ?
B20A N103 1.574(18) . ?
B20A N104 1.783(17) . ?
O14A B10A 1.52(2) . ?
B10A F14B 1.38(2) . ?
B10A N102 1.521(19) . ?
B10A N101 1.60(2) . ?
B20B F14A 1.34(2) . ?
B20B N104 1.46(3) . ?
B20B N103 1.63(3) . ?
B20B O14B 1.83(3) . ?
O14B B10B 1.04(2) . ?
F10B B10B 1.46(2) . ?
B10B N101 1.60(2) . ?
B10B N102 1.69(2) . ?
B30A F32A 1.39(2) 2_767 ?
B30A N201 1.45(2) . ?
B30A F32A 1.53(2) . ?
B30A N202 1.54(2) . ?
B30A B30A 1.93(4) 2_767 ?
F32A B30A 1.39(2) 2_767 ?
O32A B30B 1.08(2) . ?
B30B F31B 1.48(3) . ?
B30B N202 1.54(3) . ?
B30B N201 1.60(2) . ?
B31B F32B 1.40(2) . ?
B31B O31D 1.42(2) 2_557 ?
B31B O31D 1.43(2) . ?
B31B N301 1.56(2) . ?
B31B N302 1.56(2) . ?
B31B F32B 1.73(2) 2_557 ?
B31B B31B 1.73(4) 2_557 ?
F32B B31B 1.73(2) 2_557 ?
O31D B31B 1.42(2) 2_557 ?
B31C F30A 1.39(2) . ?
B31C N302 1.60(3) . ?
B31C N301 1.65(2) . ?
C1 C30 1.407(11) . ?
C1 C2 1.407(13) . ?
C1 N4 1.448(11) . ?
C2 C3 1.350(12) . ?
C3 C4 1.388(13) . ?
C4 N4 1.326(10) . ?
C4 C5 1.528(13) . ?
C5 C8 1.496(14) . ?
C5 C6 1.536(13) . ?
C5 C7 1.552(13) . ?
C8 N1 1.351(10) . ?
C8 C9 1.389(13) . ?
C9 C10 1.395(13) . ?
C10 C11 1.415(12) . ?
C11 N1 1.393(12) . ?
C11 C12 1.432(12) . ?
C12 C19 1.421(12) . ?
C12 C13 1.551(13) . ?
C13 C18 1.354(12) . ?
C13 C14 1.391(13) . ?
C14 C15 1.338(14) . ?
C14 F5 1.349(11) . ?
C15 C16 1.357(14) . ?
C15 F4 1.369(11) . ?
C16 F3 1.310(11) . ?
C16 C17 1.362(14) . ?
C17 F2 1.356(11) . ?
C17 C18 1.416(13) . ?
C18 F1 1.347(10) . ?
C19 N2 1.373(12) . ?
C19 C20 1.437(12) . ?
C20 C21 1.390(11) . ?
C21 C22 1.403(13) . ?
C22 N2 1.351(10) . ?
C22 C23 1.520(11) . ?
C23 C26 1.488(13) . ?
C23 C25 1.533(12) . ?
C23 C24 1.548(13) . ?
C26 N3 1.330(10) . ?
C26 C27 1.426(13) . ?
C27 C28 1.328(13) . ?
C28 C29 1.461(11) . ?
C29 C30 1.368(12) . ?
C29 N3 1.428(11) . ?
C30 C31 1.500(13) . ?
C31 C36 1.372(12) . ?
C31 C32 1.381(13) . ?
C32 F6 1.346(10) . ?
C32 C33 1.419(13) . ?
C33 F7 1.327(11) . ?
C33 C34 1.375(13) . ?
C34 C35 1.365(13) . ?
C34 F8 1.395(11) . ?
C35 C36 1.344(13) . ?
C35 F9 1.344(10) . ?
C36 F10 1.332(11) . ?
C301 C302 1.574(14) . ?
C302 C304 1.472(13) . ?
C302 C312 1.511(14) . ?
C302 C303 1.554(12) . ?
C304 N302 1.341(10) . ?
C304 C305 1.365(13) . ?
C305 C306 1.358(12) . ?
C306 C307 1.391(13) . ?
C307 N302 1.415(11) . ?
C307 C308 1.426(11) . ?
C308 C309 1.447(13) 2_557 ?
C308 C313 1.487(13) . ?
C309 N301 1.382(12) . ?
C309 C310 1.392(12) . ?
C309 C308 1.447(13) 2_557 ?
C310 C311 1.352(13) . ?
C311 C312 1.401(13) . ?
C312 N301 1.328(10) . ?
C313 C318 1.383(12) . ?
C313 C314 1.428(13) . ?
C314 F305 1.363(11) . ?
C314 C315 1.366(14) . ?
C315 F304 1.333(11) . ?
C315 C316 1.383(14) . ?
C316 F303 1.317(11) . ?
C316 C317 1.398(14) . ?
C317 F302 1.324(11) . ?
C317 C318 1.362(14) . ?
C318 F301 1.357(10) . ?
C101 C130 1.389(12) . ?
C101 N101 1.397(11) . ?
C101 C102 1.436(12) . ?
C102 C103 1.346(13) . ?
C103 C104 1.453(13) . ?
C104 N101 1.325(10) . ?
C104 C105 1.512(13) . ?
C105 C107 1.502(11) . ?
C105 C108 1.511(13) . ?
C105 C106 1.529(13) . ?
C108 N102 1.344(10) . ?
C108 C109 1.417(13) . ?
C109 C110 1.381(13) . ?
C110 C111 1.431(12) . ?
C111 N102 1.391(11) . ?
C111 C112 1.391(13) . ?
C112 C119 1.434(12) . ?
C112 C113 1.510(14) . ?
C113 C118 1.354(14) . ?
C113 C114 1.414(13) . ?
C114 F101 1.336(10) . ?
C114 C115 1.354(13) . ?
C115 F102 1.337(10) . ?
C115 C116 1.439(14) . ?
C116 C117 1.348(13) . ?
C116 F103 1.352(11) . ?
C117 F104 1.336(11) . ?
C117 C118 1.379(13) . ?
C118 F105 1.348(10) . ?
C119 N103 1.399(11) . ?
C119 C120 1.437(12) . ?
C120 C121 1.391(12) . ?
C121 C122 1.399(13) . ?
C122 N103 1.337(10) . ?
C122 C123 1.507(13) . ?
C123 C126 1.520(13) . ?
C123 C125 1.540(11) . ?
C123 C124 1.553(12) . ?
C126 N104 1.331(11) . ?
C126 C127 1.369(13) . ?
C127 C128 1.345(12) . ?
C128 C129 1.415(12) . ?
C129 N104 1.402(12) . ?
C129 C130 1.425(12) . ?
C130 C131 1.488(14) . ?
C131 C132 1.401(13) . ?
C131 C136 1.409(14) . ?
C132 F106 1.353(12) . ?
C132 C133 1.406(14) . ?
C133 C134 1.305(14) . ?
C133 F107 1.351(10) . ?
C134 F108 1.386(12) . ?
C134 C135 1.406(14) . ?
C135 F109 1.334(11) . ?
C135 C136 1.377(14) . ?
C136 F110 1.313(10) . ?
C201 C203 1.575(11) . ?
C202 C203 1.563(12) . ?
C203 C204 1.504(13) . ?
C203 C212 1.528(13) . ?
C204 N201 1.358(11) . ?
C204 C205 1.413(12) . ?
C205 C206 1.402(13) . ?
C206 C207 1.394(13) . ?
C207 N201 1.394(12) . ?
C207 C208 1.471(12) . ?
C208 C209 1.400(12) 2_767 ?
C208 C213 1.497(13) . ?
C209 C208 1.400(12) 2_767 ?
C209 C210 1.408(12) . ?
C209 N202 1.430(12) . ?
C210 C211 1.352(13) . ?
C211 C212 1.351(13) . ?
C212 N202 1.358(11) . ?
C213 C214 1.364(13) . ?
C213 C218 1.409(13) . ?
C214 C215 1.351(14) . ?
C214 F201 1.355(11) . ?
C215 F202 1.330(11) . ?
C215 C216 1.378(15) . ?
C216 F203 1.297(11) . ?
C216 C217 1.379(13) . ?
C217 F204 1.351(11) . ?
C217 C218 1.361(14) . ?
C218 F205 1.356(10) . ?

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
O1E B1A F1F 114.3(16) . . ?
O1E B1A N1 115.3(15) . . ?
F1F B1A N1 105.5(14) . . ?
O1E B1A N4 107.9(15) . . ?
F1F B1A N4 107.1(14) . . ?
N1 B1A N4 106.3(12) . . ?
B1A O1E B2A 121.9(17) . . ?
F2A B2A O1E 115.2(19) . . ?
F2A B2A N2 113.9(17) . . ?
O1E B2A N2 112.2(15) . . ?
F2A B2A N3 110.4(15) . . ?
O1E B2A N3 104.2(15) . . ?
N2 B2A N3 99.4(13) . . ?
O1F B1B F1B 111.1(19) . . ?
O1F B1B N1 115.5(18) . . ?
F1B B1B N1 113.9(14) . . ?
O1F B1B N4 109.2(17) . . ?
F1B B1B N4 104.4(15) . . ?
N1 B1B N4 101.6(13) . . ?
B1B O1F B2B 122(2) . . ?
O1F B2B F1E 113.3(19) . . ?
O1F B2B N2 113(2) . . ?
F1E B2B N2 104.7(16) . . ?
O1F B2B N3 111.5(19) . . ?
F1E B2B N3 105.3(16) . . ?
N2 B2B N3 108.2(15) . . ?
F11A B20A O14A 109.8(12) . . ?
F11A B20A N103 116.9(12) . . ?
O14A B20A N103 111.7(13) . . ?
F11A B20A N104 113.4(12) . . ?
O14A B20A N104 109.5(12) . . ?
N103 B20A N104 94.6(9) . . ?
B20A O14A B10A 118.8(13) . . ?
F14B B10A O14A 101.7(13) . . ?
F14B B10A N102 116.6(15) . . ?
O14A B10A N102 106.5(12) . . ?
F14B B10A N101 113.0(13) . . ?
O14A B10A N101 111.6(14) . . ?
N102 B10A N101 107.2(12) . . ?
F14A B20B N104 104.8(19) . . ?
F14A B20B N103 107.3(16) . . ?
N104 B20B N103 106.1(16) . . ?
F14A B20B O14B 110.9(17) . . ?
N104 B20B O14B 117.8(15) . . ?
N103 B20B O14B 109.4(16) . . ?
B10B O14B B20B 106.3(17) . . ?
O14B B10B F10B 92.3(17) . . ?
O14B B10B N101 127.1(19) . . ?
F10B B10B N101 107.6(13) . . ?
O14B B10B N102 119.8(18) . . ?
F10B B10B N102 109.0(13) . . ?
N101 B10B N102 99.6(11) . . ?
F32A B30A N201 116.8(15) 2_767 . ?
F32A B30A F32A 97.1(14) 2_767 . ?
N201 B30A F32A 113.7(16) . . ?
F32A B30A N202 111.7(16) 2_767 . ?
N201 B30A N202 110.5(14) . . ?
F32A B30A N202 106.0(13) . . ?
F32A B30A B30A 51.7(11) 2_767 2_767 ?
N201 B30A B30A 130(2) . 2_767 ?
F32A B30A B30A 45.4(9) . 2_767 ?
N202 B30A B30A 118.9(18) . 2_767 ?
B30A F32A B30A 82.9(14) 2_767 . ?
O32A B30B F31B 89.0(19) . . ?
O32A B30B N202 127(2) . . ?
F31B B30B N202 107.2(16) . . ?
O32A B30B N201 116(2) . . ?
F31B B30B N201 114.5(17) . . ?
N202 B30B N201 103.0(15) . . ?
F32B B31B O31D 118.7(16) . 2_557 ?
O31D B31B O31D 105.1(14) 2_557 . ?
F32B B31B N301 105.9(14) . . ?
O31D B31B N301 109.4(14) 2_557 . ?
O31D B31B N301 114.6(15) . . ?
F32B B31B N302 106.7(14) . . ?
O31D B31B N302 109.8(15) 2_557 . ?
O31D B31B N302 112.4(14) . . ?
N301 B31B N302 105.6(12) . . ?
F32B B31B F32B 113.8(13) . 2_557 ?
O31D B31B F32B 100.2(13) . 2_557 ?
N301 B31B F32B 113.2(13) . 2_557 ?
N302 B31B F32B 111.1(13) . 2_557 ?
F32B B31B B31B 65.9(14) . 2_557 ?
O31D B31B B31B 52.8(12) 2_557 2_557 ?
O31D B31B B31B 52.3(12) . 2_557 ?
N301 B31B B31B 128(2) . 2_557 ?
N302 B31B B31B 126.3(19) . 2_557 ?
F32B B31B B31B 47.9(10) 2_557 2_557 ?
B31B F32B B31B 66.2(13) . 2_557 ?
B31B O31D B31B 74.9(14) 2_557 . ?
F30A B31C N302 112.1(16) . . ?
F30A B31C N301 107.8(14) . . ?
N302 B31C N301 99.7(13) . . ?
C30 C1 C2 125.8(9) . . ?
C30 C1 N4 130.4(9) . . ?
C2 C1 N4 103.7(7) . . ?
C3 C2 C1 110.1(10) . . ?
C2 C3 C4 107.7(9) . . ?
N4 C4 C3 109.7(8) . . ?
N4 C4 C5 122.9(9) . . ?
C3 C4 C5 127.4(8) . . ?
C8 C5 C4 112.0(7) . . ?
C8 C5 C6 109.0(8) . . ?
C4 C5 C6 107.2(8) . . ?
C8 C5 C7 109.9(9) . . ?
C4 C5 C7 106.6(8) . . ?
C6 C5 C7 112.2(8) . . ?
N1 C8 C9 110.2(9) . . ?
N1 C8 C5 123.1(9) . . ?
C9 C8 C5 126.7(9) . . ?
C8 C9 C10 105.9(8) . . ?
C9 C10 C11 109.1(9) . . ?
N1 C11 C10 105.6(8) . . ?
N1 C11 C12 131.4(8) . . ?
C10 C11 C12 123.0(9) . . ?
C19 C12 C11 136.9(9) . . ?
C19 C12 C13 110.9(8) . . ?
C11 C12 C13 112.1(7) . . ?
C18 C13 C14 119.4(10) . . ?
C18 C13 C12 119.6(9) . . ?
C14 C13 C12 121.0(9) . . ?
C15 C14 F5 120.5(10) . . ?
C15 C14 C13 119.6(10) . . ?
F5 C14 C13 119.8(10) . . ?
C14 C15 C16 123.3(10) . . ?
C14 C15 F4 118.8(11) . . ?
C16 C15 F4 117.7(10) . . ?
F3 C16 C15 124.0(10) . . ?
F3 C16 C17 118.4(11) . . ?
C15 C16 C17 117.5(10) . . ?
F2 C17 C16 122.4(10) . . ?
F2 C17 C18 116.6(10) . . ?
C16 C17 C18 121.0(10) . . ?
F1 C18 C13 121.9(9) . . ?
F1 C18 C17 119.1(9) . . ?
C13 C18 C17 119.0(10) . . ?
N2 C19 C12 130.7(9) . . ?
N2 C19 C20 108.0(8) . . ?
C12 C19 C20 121.3(9) . . ?
C21 C20 C19 106.2(8) . . ?
C20 C21 C22 107.4(8) . . ?
N2 C22 C21 109.7(8) . . ?
N2 C22 C23 122.7(9) . . ?
C21 C22 C23 127.6(8) . . ?
C26 C23 C22 112.7(7) . . ?
C26 C23 C25 109.6(8) . . ?
C22 C23 C25 107.4(8) . . ?
C26 C23 C24 108.5(8) . . ?
C22 C23 C24 108.6(8) . . ?
C25 C23 C24 110.0(8) . . ?
N3 C26 C27 107.5(9) . . ?
N3 C26 C23 123.7(9) . . ?
C27 C26 C23 128.7(8) . . ?
C28 C27 C26 109.8(9) . . ?
C27 C28 C29 108.1(9) . . ?
C30 C29 N3 131.9(8) . . ?
C30 C29 C28 123.9(9) . . ?
N3 C29 C28 104.0(8) . . ?
C29 C30 C1 138.5(9) . . ?
C29 C30 C31 112.0(8) . . ?
C1 C30 C31 109.5(8) . . ?
C36 C31 C32 116.1(10) . . ?
C36 C31 C30 123.6(10) . . ?
C32 C31 C30 120.2(9) . . ?
F6 C32 C31 121.5(10) . . ?
F6 C32 C33 115.7(10) . . ?
C31 C32 C33 122.8(10) . . ?
F7 C33 C34 122.2(10) . . ?
F7 C33 C32 121.9(9) . . ?
C34 C33 C32 115.8(10) . . ?
C35 C34 C33 122.5(10) . . ?
C35 C34 F8 120.5(9) . . ?
C33 C34 F8 116.9(10) . . ?
C36 C35 F9 123.5(9) . . ?
C36 C35 C34 119.0(9) . . ?
F9 C35 C34 117.5(9) . . ?
F10 C36 C35 117.3(9) . . ?
F10 C36 C31 118.9(10) . . ?
C35 C36 C31 123.7(10) . . ?
C8 N1 C11 109.2(8) . . ?
C8 N1 B1B 113.6(11) . . ?
C11 N1 B1B 128.5(11) . . ?
C8 N1 B1A 126.8(11) . . ?
C11 N1 B1A 122.9(10) . . ?
C22 N2 C19 108.6(9) . . ?
C22 N2 B2B 125.7(11) . . ?
C19 N2 B2B 124.6(11) . . ?
C22 N2 B2A 110.0(10) . . ?
C19 N2 B2A 131.0(10) . . ?
C26 N3 C29 110.5(8) . . ?
C26 N3 B2B 125.3(12) . . ?
C29 N3 B2B 123.4(11) . . ?
C26 N3 B2A 109.8(10) . . ?
C29 N3 B2A 129.5(11) . . ?
C4 N4 C1 108.7(8) . . ?
C4 N4 B1A 127.1(10) . . ?
C1 N4 B1A 122.7(9) . . ?
C4 N4 B1B 113.0(10) . . ?
C1 N4 B1B 131.7(10) . . ?
C304 C302 C312 115.1(8) . . ?
C304 C302 C303 109.4(9) . . ?
C312 C302 C303 107.5(9) . . ?
C304 C302 C301 109.3(9) . . ?
C312 C302 C301 108.5(8) . . ?
C303 C302 C301 106.7(9) . . ?
N302 C304 C305 109.4(8) . . ?
N302 C304 C302 121.1(10) . . ?
C305 C304 C302 129.4(9) . . ?
C306 C305 C304 109.0(9) . . ?
C305 C306 C307 107.4(10) . . ?
C306 C307 N302 106.8(8) . . ?
C306 C307 C308 123.7(9) . . ?
N302 C307 C308 129.3(9) . . ?
C307 C308 C309 138.9(10) . 2_557 ?
C307 C308 C313 110.4(9) . . ?
C309 C308 C313 110.7(8) 2_557 . ?
N301 C309 C310 107.3(8) . . ?
N301 C309 C308 129.9(8) . 2_557 ?
C310 C309 C308 122.8(9) . 2_557 ?
C311 C310 C309 107.8(9) . . ?
C310 C311 C312 107.6(9) . . ?
N301 C312 C311 108.6(9) . . ?
N301 C312 C302 121.7(8) . . ?
C311 C312 C302 129.7(9) . . ?
C318 C313 C314 112.8(9) . . ?
C318 C313 C308 124.5(8) . . ?
C314 C313 C308 122.7(9) . . ?
F305 C314 C315 118.2(9) . . ?
F305 C314 C313 117.5(9) . . ?
C315 C314 C313 124.2(10) . . ?
F304 C315 C314 120.0(10) . . ?
F304 C315 C316 120.8(10) . . ?
C314 C315 C316 119.2(10) . . ?
F303 C316 C315 120.4(10) . . ?
F303 C316 C317 120.3(11) . . ?
C315 C316 C317 119.2(10) . . ?
F302 C317 C318 121.4(10) . . ?
F302 C317 C316 119.3(11) . . ?
C318 C317 C316 119.1(11) . . ?
F301 C318 C317 117.0(9) . . ?
F301 C318 C313 117.6(9) . . ?
C317 C318 C313 125.3(10) . . ?
C312 N301 C309 108.7(8) . . ?
C312 N301 B31B 127.3(11) . . ?
C309 N301 B31B 123.3(10) . . ?
C312 N301 B31C 112.1(11) . . ?
C309 N301 B31C 130.7(11) . . ?
C304 N302 C307 107.3(8) . . ?
C304 N302 B31B 128.2(10) . . ?
C307 N302 B31B 123.8(9) . . ?
C304 N302 B31C 113.2(10) . . ?
C307 N302 B31C 129.7(10) . . ?
C130 C101 N101 131.5(9) . . ?
C130 C101 C102 123.7(9) . . ?
N101 C101 C102 104.9(8) . . ?
C103 C102 C101 109.5(10) . . ?
C102 C103 C104 106.6(9) . . ?
N101 C104 C103 107.9(9) . . ?
N101 C104 C105 124.1(9) . . ?
C103 C104 C105 127.9(8) . . ?
C107 C105 C108 110.1(8) . . ?
C107 C105 C104 110.3(8) . . ?
C108 C105 C104 109.5(7) . . ?
C107 C105 C106 107.7(8) . . ?
C108 C105 C106 110.8(8) . . ?
C104 C105 C106 108.3(8) . . ?
N102 C108 C109 108.1(9) . . ?
N102 C108 C105 124.3(8) . . ?
C109 C108 C105 127.6(8) . . ?
C110 C109 C108 107.0(9) . . ?
C109 C110 C111 108.7(10) . . ?
N102 C111 C112 131.4(9) . . ?
N102 C111 C110 105.0(8) . . ?
C112 C111 C110 123.6(9) . . ?
C111 C112 C119 138.7(10) . . ?
C111 C112 C113 112.5(9) . . ?
C119 C112 C113 108.8(8) . . ?
C118 C113 C114 117.0(10) . . ?
C118 C113 C112 122.3(10) . . ?
C114 C113 C112 120.6(10) . . ?
F101 C114 C115 118.8(10) . . ?
F101 C114 C113 119.6(10) . . ?
C115 C114 C113 121.5(10) . . ?
F102 C115 C114 123.2(10) . . ?
F102 C115 C116 118.1(9) . . ?
C114 C115 C116 118.7(9) . . ?
C117 C116 F103 121.0(10) . . ?
C117 C116 C115 119.9(10) . . ?
F103 C116 C115 119.1(9) . . ?
F104 C117 C116 118.7(10) . . ?
F104 C117 C118 122.1(9) . . ?
C116 C117 C118 119.2(10) . . ?
F105 C118 C113 119.0(10) . . ?
F105 C118 C117 117.4(10) . . ?
C113 C118 C117 123.6(10) . . ?
N103 C119 C112 130.9(9) . . ?
N103 C119 C120 106.4(8) . . ?
C112 C119 C120 122.7(9) . . ?
C121 C120 C119 106.8(9) . . ?
C120 C121 C122 107.8(8) . . ?
N103 C122 C121 109.3(9) . . ?
N103 C122 C123 122.2(9) . . ?
C121 C122 C123 128.2(8) . . ?
C122 C123 C126 110.7(8) . . ?
C122 C123 C125 108.8(8) . . ?
C126 C123 C125 109.9(7) . . ?
C122 C123 C124 107.4(8) . . ?
C126 C123 C124 111.9(8) . . ?
C125 C123 C124 107.9(7) . . ?
N104 C126 C127 109.9(9) . . ?
N104 C126 C123 121.3(8) . . ?
C127 C126 C123 128.8(9) . . ?
C128 C127 C126 107.5(9) . . ?
C127 C128 C129 109.3(9) . . ?
N104 C129 C128 104.4(8) . . ?
N104 C129 C130 131.7(9) . . ?
C128 C129 C130 123.8(10) . . ?
C101 C130 C129 138.7(10) . . ?
C101 C130 C131 110.1(8) . . ?
C129 C130 C131 111.2(9) . . ?
C132 C131 C136 115.5(10) . . ?
C132 C131 C130 121.3(10) . . ?
C136 C131 C130 122.9(9) . . ?
F106 C132 C131 119.7(10) . . ?
F106 C132 C133 117.7(10) . . ?
C131 C132 C133 122.6(11) . . ?
C134 C133 F107 121.6(11) . . ?
C134 C133 C132 118.4(11) . . ?
F107 C133 C132 120.0(10) . . ?
C133 C134 F108 121.1(11) . . ?
C133 C134 C135 123.5(11) . . ?
F108 C134 C135 115.4(10) . . ?
F109 C135 C136 121.1(10) . . ?
F109 C135 C134 121.4(11) . . ?
C136 C135 C134 117.6(11) . . ?
F110 C136 C135 118.2(10) . . ?
F110 C136 C131 119.5(10) . . ?
C135 C136 C131 122.3(10) . . ?
C104 N101 C101 111.0(8) . . ?
C104 N101 B10B 117.9(10) . . ?
C101 N101 B10B 126.7(9) . . ?
C104 N101 B10A 124.3(9) . . ?
C101 N101 B10A 122.5(9) . . ?
C108 N102 C111 111.1(8) . . ?
C108 N102 B10A 125.0(10) . . ?
C111 N102 B10A 120.2(10) . . ?
C108 N102 B10B 115.8(10) . . ?
C111 N102 B10B 130.8(9) . . ?
C122 N103 C119 109.5(8) . . ?
C122 N103 B20A 115.8(9) . . ?
C119 N103 B20A 126.6(8) . . ?
C122 N103 B20B 123.9(11) . . ?
C119 N103 B20B 123.6(11) . . ?
C126 N104 C129 108.9(8) . . ?
C126 N104 B20B 128.6(13) . . ?
C129 N104 B20B 118.0(12) . . ?
C126 N104 B20A 113.9(8) . . ?
C129 N104 B20A 133.4(8) . . ?
C204 C203 C212 113.6(8) . . ?
C204 C203 C202 109.8(8) . . ?
C212 C203 C202 107.3(7) . . ?
C204 C203 C201 108.4(7) . . ?
C212 C203 C201 110.5(8) . . ?
C202 C203 C201 106.9(7) . . ?
N201 C204 C205 109.9(8) . . ?
N201 C204 C203 120.8(8) . . ?
C205 C204 C203 129.3(8) . . ?
C206 C205 C204 106.5(8) . . ?
C207 C206 C205 107.0(9) . . ?
C206 C207 N201 109.4(9) . . ?
C206 C207 C208 121.3(10) . . ?
N201 C207 C208 129.3(9) . . ?
C209 C208 C207 137.8(10) 2_767 . ?
C209 C208 C213 110.9(8) 2_767 . ?
C207 C208 C213 111.2(8) . . ?
C208 C209 C210 124.1(10) 2_767 . ?
C208 C209 N202 129.8(9) 2_767 . ?
C210 C209 N202 106.2(8) . . ?
C211 C210 C209 109.1(10) . . ?
C212 C211 C210 107.2(9) . . ?
C211 C212 N202 112.4(8) . . ?
C211 C212 C203 129.0(9) . . ?
N202 C212 C203 118.6(9) . . ?
C214 C213 C218 116.5(10) . . ?
C214 C213 C208 124.3(10) . . ?
C218 C213 C208 119.0(9) . . ?
C215 C214 F201 118.6(9) . . ?
C215 C214 C213 123.5(10) . . ?
F201 C214 C213 117.9(10) . . ?
F202 C215 C214 120.3(11) . . ?
F202 C215 C216 119.2(11) . . ?
C214 C215 C216 120.4(10) . . ?
F203 C216 C215 120.9(10) . . ?
F203 C216 C217 121.8(10) . . ?
C215 C216 C217 117.3(11) . . ?
F204 C217 C218 119.6(10) . . ?
F204 C217 C216 118.0(11) . . ?
C218 C217 C216 122.4(11) . . ?
F205 C218 C217 120.1(10) . . ?
F205 C218 C213 119.8(10) . . ?
C217 C218 C213 119.8(10) . . ?
C204 N201 C207 107.1(8) . . ?
C204 N201 B30A 124.4(11) . . ?
C207 N201 B30A 122.4(11) . . ?
C204 N201 B30B 115.5(11) . . ?
C207 N201 B30B 135.0(12) . . ?
C212 N202 C209 105.1(8) . . ?
C212 N202 B30A 124.7(10) . . ?
C209 N202 B30A 126.3(10) . . ?
C212 N202 B30B 117.3(12) . . ?
C209 N202 B30B 132.4(11) . . ?

_refine_diff_density_max         0.530
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.064

