# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_132JART13
_database_code_depnum_ccdc_archive 'CCDC 1544788'
_audit_update_record             
;
2017-04-18 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_audit_creation_date             13-11-11
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title '132jart13 in P-1'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   12.7841(7)
_cell_length_b                   13.6797(8)
_cell_length_c                   19.6984(11)
_cell_angle_alpha                102.002(5)
_cell_angle_beta                 98.529(5)
_cell_angle_gamma                110.113(5)
_cell_volume                     3072.2(3)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Al 0.2130 0.2455 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886
1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
K 0.3868 1.0657 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C49 H60 Al1 B0.50 Cl1 F15 K0.50 N2 O1 
# Dc =      1.15 Fooo =   1284.00 Mu =     16.76 M =   1065.39
# Found Formula = C59 H69 Al1 B1 Cl1 F15 K1 N2 O2 
# Dc =      1.34 FOOO =   1284.00 Mu =     20.62 M =   1235.52

_chemical_formula_sum            'C59 H69 Al1 B1 Cl1 F15 K1 N2 O2'
_chemical_formula_moiety         'C59 H69 Al1 B1 Cl1 F15 K1 N2 O2'
_chemical_compound_source        .
_chemical_formula_weight         1235.52


_cell_measurement_reflns_used    9430
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_max          0.210

_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1284
_exptl_absorpt_coefficient_mu    2.062

# Sheldrick geometric approximatio 0.69 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.90
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            32711
_reflns_number_total             12645
_diffrn_reflns_av_R_equivalents  0.056
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 12645 
# Theoretical number of reflections is about 25763 


_diffrn_reflns_theta_min         3.583
_diffrn_reflns_theta_max         76.311
_diffrn_measured_fraction_theta_max 0.982

_diffrn_reflns_theta_full        73.258
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              -17
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   3.28
_oxford_diffrn_Wilson_scale      0.04

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.96
_refine_diff_density_max         1.98


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         12594
_refine_ls_number_restraints     68
_refine_ls_number_parameters     767
_oxford_refine_ls_R_factor_ref   0.0967
_refine_ls_wR_factor_ref         0.2050
_refine_ls_goodness_of_fit_ref   0.9985
_refine_ls_shift/su_max          0.0005484
_refine_ls_shift/su_mean         0.0000308


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        12596
_refine_ls_R_factor_all          0.0967
_refine_ls_wR_factor_all         0.2051

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8954
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_gt          0.1883

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 8.56P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Al1 Al 0.79248(10) 0.72482(10) 0.20924(6) 0.0359 1.0000 Uani . . . . . .
Cl2 Cl 0.65671(9) 0.59730(9) 0.23266(6) 0.0499 1.0000 Uani . . . . . .
K3 K 0.63221(11) 0.37919(9) 0.26037(7) 0.0644 1.0000 Uani . . . . . .
N4 N 0.8917(3) 0.6559(2) 0.18179(15) 0.0287 1.0000 Uani . . . . . .
C5 C 0.9579(3) 0.6352(3) 0.23205(18) 0.0266 1.0000 Uani . . . . . .
C6 C 1.0166(3) 0.5583(3) 0.21079(19) 0.0300 1.0000 Uani . . . . . .
C7 C 0.9755(3) 0.6854(3) 0.30526(18) 0.0289 1.0000 Uani . . . . . .
C8 C 0.9497(3) 0.7724(3) 0.33736(19) 0.0296 1.0000 Uani . . . . . .
C9 C 0.9986(4) 0.8209(3) 0.41640(19) 0.0373 1.0000 Uani . . . . . .
N10 N 0.8852(3) 0.8135(2) 0.30074(16) 0.0320 1.0000 Uani . . . . . .
C11 C 0.8775(4) 0.9137(3) 0.3373(2) 0.0391 1.0000 Uani . . . . . .
C12 C 0.7968(4) 0.9134(4) 0.3776(2) 0.0440 1.0000 Uani . . . . . .
C13 C 0.7183(4) 0.8116(4) 0.3919(2) 0.0503 1.0000 Uani . . . . . .
C14 C 0.7388(5) 0.8224(5) 0.4726(3) 0.0603 1.0000 Uani . . . . . .
C15 C 0.5923(4) 0.7876(5) 0.3616(3) 0.0617 1.0000 Uani . . . . . .
C16 C 0.7910(5) 1.0134(4) 0.4087(2) 0.0578 1.0000 Uani . . . . . .
C17 C 0.8642(5) 1.1082(4) 0.4013(3) 0.0640 1.0000 Uani . . . . . .
C18 C 0.9467(5) 1.1086(4) 0.3641(3) 0.0583 1.0000 Uani . . . . . .
C19 C 0.9562(4) 1.0123(3) 0.3307(2) 0.0461 1.0000 Uani . . . . . .
C20 C 1.0487(4) 1.0142(4) 0.2905(2) 0.0503 1.0000 Uani . . . . . .
C21 C 1.0824(6) 1.1087(5) 0.2566(3) 0.0792 1.0000 Uani . . . . . .
C22 C 1.1569(5) 1.0173(5) 0.3370(3) 0.0616 1.0000 Uani . . . . . .
C23 C 0.8896(3) 0.6169(3) 0.10689(19) 0.0309 1.0000 Uani . . . . . .
C24 C 0.8180(3) 0.5102(3) 0.0665(2) 0.0356 1.0000 Uani . . . . . .
C25 C 0.7366(3) 0.4281(3) 0.0959(2) 0.0397 1.0000 Uani . . . . . .
C26 C 0.6113(4) 0.4110(4) 0.0672(3) 0.0551 1.0000 Uani . . . . . .
C27 C 0.7497(4) 0.3192(3) 0.0789(3) 0.0509 1.0000 Uani . . . . . .
C28 C 0.8192(4) 0.4786(4) -0.0054(2) 0.0431 1.0000 Uani . . . . . .
C29 C 0.8885(4) 0.5482(4) -0.0362(2) 0.0485 1.0000 Uani . . . . . .
C30 C 0.9569(4) 0.6538(3) 0.0040(2) 0.0421 1.0000 Uani . . . . . .
C31 C 0.9567(3) 0.6909(3) 0.0747(2) 0.0354 1.0000 Uani . . . . . .
C32 C 1.0268(4) 0.8092(3) 0.1154(2) 0.0410 1.0000 Uani . . . . . .
C33 C 1.1423(4) 0.8252(4) 0.1591(3) 0.0546 1.0000 Uani . . . . . .
C34 C 1.0419(5) 0.8854(4) 0.0669(3) 0.0579 1.0000 Uani . . . . . .
C35 C 0.7208(4) 0.7916(4) 0.1439(2) 0.0500 1.0000 Uani . . . . . .
C36 C 0.7973(5) 0.9090(4) 0.1473(3) 0.0644 1.0000 Uani . . . . . .
C37 C 0.6127(5) 0.7973(6) 0.1653(3) 0.0777 1.0000 Uani . . . . . .
C38 C 0.6877(5) 0.7236(4) 0.0660(2) 0.0578 1.0000 Uani . . . . . .
B39 B 1.1156(4) 0.5453(3) 0.2687(2) 0.0300 1.0000 Uani . . . . . .
C40 C 1.2210(3) 0.6665(3) 0.2982(2) 0.0323 1.0000 Uani . . . . . .
C41 C 1.2517(3) 0.7393(3) 0.3654(2) 0.0385 1.0000 Uani . . . . . .
F42 F 1.2027(2) 0.7095(2) 0.41863(12) 0.0456 1.0000 Uani . . . . . .
C43 C 1.3282(4) 0.8458(3) 0.3838(3) 0.0475 1.0000 Uani . . . . . .
F44 F 1.3507(3) 0.9123(2) 0.44989(16) 0.0639 1.0000 Uani . . . . . .
C45 C 1.3823(4) 0.8851(3) 0.3342(3) 0.0507 1.0000 Uani . . . . . .
F46 F 1.4586(3) 0.9878(2) 0.3506(2) 0.0716 1.0000 Uani . . . . . .
C47 C 1.3589(3) 0.8169(3) 0.2668(3) 0.0450 1.0000 Uani . . . . . .
F48 F 1.4102(2) 0.8536(2) 0.21732(17) 0.0593 1.0000 Uani . . . . . .
C49 C 1.2798(3) 0.7112(3) 0.2506(2) 0.0372 1.0000 Uani . . . . . .
F50 F 1.2592(2) 0.65073(18) 0.18283(13) 0.0422 1.0000 Uani . . . . . .
C51 C 1.1559(3) 0.4508(3) 0.2254(2) 0.0323 1.0000 Uani . . . . . .
C52 C 1.2655(3) 0.4576(3) 0.2215(2) 0.0381 1.0000 Uani . . . . . .
F53 F 1.3583(2) 0.54898(19) 0.25779(15) 0.0490 1.0000 Uani . . . . . .
C54 C 1.2902(4) 0.3756(4) 0.1828(3) 0.0455 1.0000 Uani . . . . . .
F55 F 1.4001(2) 0.3887(2) 0.18266(19) 0.0662 1.0000 Uani . . . . . .
C56 C 1.2031(4) 0.2780(3) 0.1445(2) 0.0449 1.0000 Uani . . . . . .
F57 F 1.2254(3) 0.1982(2) 0.10557(17) 0.0635 1.0000 Uani . . . . . .
C58 C 1.0928(4) 0.2641(3) 0.1482(2) 0.0387 1.0000 Uani . . . . . .
F59 F 1.0054(2) 0.16889(18) 0.11279(13) 0.0469 1.0000 Uani . . . . . .
C60 C 1.0727(3) 0.3471(3) 0.1890(2) 0.0333 1.0000 Uani . . . . . .
F61 F 0.96193(19) 0.32350(17) 0.19336(13) 0.0405 1.0000 Uani . . . . . .
C62 C 1.0720(4) 0.4949(3) 0.3339(2) 0.0367 1.0000 Uani . . . . . .
C63 C 0.9605(4) 0.4498(3) 0.3404(2) 0.0414 1.0000 Uani . . . . . .
F64 F 0.8718(2) 0.44802(19) 0.29199(14) 0.0457 1.0000 Uani . . . . . .
C65 C 0.9297(5) 0.4053(4) 0.3950(3) 0.0561 1.0000 Uani . . . . . .
F66 F 0.8182(3) 0.3679(2) 0.39812(17) 0.0726 1.0000 Uani . . . . . .
C67 C 1.0108(6) 0.4009(4) 0.4456(3) 0.0631 1.0000 Uani . . . . . .
F68 F 0.9833(4) 0.3594(2) 0.49970(17) 0.0877 1.0000 Uani . . . . . .
C69 C 1.1231(6) 0.4403(4) 0.4412(2) 0.0621 1.0000 Uani . . . . . .
F70 F 1.2052(4) 0.4355(3) 0.49040(17) 0.0875 1.0000 Uani . . . . . .
C71 C 1.1508(4) 0.4859(4) 0.3864(2) 0.0476 1.0000 Uani . . . . . .
F72 F 1.2631(3) 0.5234(2) 0.38567(15) 0.0604 1.0000 Uani . . . . . .
C73 C 0.7243(6) 0.1581(5) 0.2417(4) 0.0787 1.0000 Uani . . . . . .
C74 C 0.6095(5) 0.0975(4) 0.1925(4) 0.0750 1.0000 Uani . . . . . .
O75 O 0.5509(3) 0.1685(3) 0.1901(3) 0.0817 1.0000 Uani D . . . . .
C76 C 0.4289(8) 0.1044(17) 0.1704(11) 0.0980 0.48(3) Uani D . P 1 1 .
C77 C 0.3921(16) 0.0546(19) 0.0901(12) 0.1105 0.48(3) Uani D . P 1 1 .
C78 C 0.4319(8) 0.1221(19) 0.1507(10) 0.1053 0.52(3) Uani D . P 1 2 .
C79 C 0.427(2) 0.0852(19) 0.0721(9) 0.1169 0.52(3) Uani D . P 1 2 .
C80 C 0.4948(6) 0.2320(5) 0.3791(4) 0.0807 1.0000 Uani . . . . . .
C81 C 0.5619(6) 0.2389(5) 0.4495(3) 0.0826 1.0000 Uani . . . . . .
O82 O 0.5255(3) 0.3345(3) 0.3640(2) 0.0679 1.0000 Uani D . . . . .
C83 C 0.499(2) 0.4104(10) 0.4131(9) 0.0746 0.52(3) Uani D . P 1 2 .
C84 C 0.4624(14) 0.3967(8) 0.3887(16) 0.0818 0.48(3) Uani D . P 1 1 .
C85 C 0.5264(6) 0.5119(5) 0.3909(4) 0.0834 1.0000 Uani D . . . . .
H61 H 1.0517 0.5794 0.1719 0.0382 1.0000 Uiso R . . . . .
H62 H 0.9544 0.4861 0.1903 0.0385 1.0000 Uiso R . . . . .
H71 H 1.0113 0.6572 0.3368 0.0363 1.0000 Uiso R . . . . .
H91 H 1.0148 0.8975 0.4306 0.0597 1.0000 Uiso R . . . . .
H92 H 1.0680 0.8102 0.4303 0.0599 1.0000 Uiso R . . . . .
H93 H 0.9450 0.7866 0.4421 0.0598 1.0000 Uiso R . . . . .
H131 H 0.7377 0.7513 0.3679 0.0606 1.0000 Uiso R . . . . .
H141 H 0.6974 0.7527 0.4800 0.0949 1.0000 Uiso R . . . . .
H142 H 0.8205 0.8465 0.4928 0.0950 1.0000 Uiso R . . . . .
H143 H 0.7101 0.8746 0.4947 0.0950 1.0000 Uiso R . . . . .
H151 H 0.5453 0.7198 0.3698 0.0955 1.0000 Uiso R . . . . .
H152 H 0.5719 0.8450 0.3870 0.0959 1.0000 Uiso R . . . . .
H153 H 0.5772 0.7816 0.3108 0.0955 1.0000 Uiso R . . . . .
H161 H 0.7352 1.0147 0.4346 0.0757 1.0000 Uiso R . . . . .
H171 H 0.8567 1.1737 0.4218 0.0777 1.0000 Uiso R . . . . .
H181 H 0.9984 1.1749 0.3611 0.0713 1.0000 Uiso R . . . . .
H201 H 1.0177 0.9467 0.2506 0.0619 1.0000 Uiso R . . . . .
H211 H 1.1280 1.0961 0.2235 0.1219 1.0000 Uiso R . . . . .
H212 H 1.1260 1.1748 0.2945 0.1218 1.0000 Uiso R . . . . .
H213 H 1.0124 1.1115 0.2323 0.1219 1.0000 Uiso R . . . . .
H223 H 1.2131 1.0179 0.3088 0.0946 1.0000 Uiso R . . . . .
H222 H 1.1873 1.0813 0.3774 0.0950 1.0000 Uiso R . . . . .
H221 H 1.1407 0.9542 0.3544 0.0950 1.0000 Uiso R . . . . .
H251 H 0.7541 0.4572 0.1493 0.0506 1.0000 Uiso R . . . . .
H263 H 0.5622 0.3607 0.0894 0.0862 1.0000 Uiso R . . . . .
H262 H 0.6045 0.4800 0.0808 0.0861 1.0000 Uiso R . . . . .
H261 H 0.5912 0.3822 0.0156 0.0859 1.0000 Uiso R . . . . .
H271 H 0.7027 0.2736 0.1032 0.0810 1.0000 Uiso R . . . . .
H272 H 0.8295 0.3281 0.0937 0.0812 1.0000 Uiso R . . . . .
H273 H 0.7222 0.2850 0.0273 0.0804 1.0000 Uiso R . . . . .
H281 H 0.7704 0.4077 -0.0330 0.0536 1.0000 Uiso R . . . . .
H291 H 0.8902 0.5245 -0.0847 0.0601 1.0000 Uiso R . . . . .
H301 H 1.0044 0.7017 -0.0176 0.0523 1.0000 Uiso R . . . . .
H321 H 0.9837 0.8310 0.1495 0.0521 1.0000 Uiso R . . . . .
H331 H 1.1859 0.9020 0.1844 0.0840 1.0000 Uiso R . . . . .
H332 H 1.1833 0.7995 0.1256 0.0835 1.0000 Uiso R . . . . .
H333 H 1.1298 0.7832 0.1938 0.0840 1.0000 Uiso R . . . . .
H341 H 1.0729 0.9595 0.0969 0.0920 1.0000 Uiso R . . . . .
H342 H 1.0940 0.8733 0.0376 0.0918 1.0000 Uiso R . . . . .
H343 H 0.9676 0.8706 0.0364 0.0922 1.0000 Uiso R . . . . .
H361 H 0.8675 0.9097 0.1319 0.0992 1.0000 Uiso R . . . . .
H362 H 0.8171 0.9550 0.1964 0.0989 1.0000 Uiso R . . . . .
H363 H 0.7531 0.9352 0.1154 0.0990 1.0000 Uiso R . . . . .
H373 H 0.5621 0.7211 0.1618 0.1163 1.0000 Uiso R . . . . .
H372 H 0.6341 0.8436 0.2143 0.1170 1.0000 Uiso R . . . . .
H371 H 0.5757 0.8260 0.1326 0.1171 1.0000 Uiso R . . . . .
H381 H 0.6381 0.6497 0.0614 0.0901 1.0000 Uiso R . . . . .
H382 H 0.7578 0.7251 0.0510 0.0901 1.0000 Uiso R . . . . .
H383 H 0.6483 0.7546 0.0367 0.0896 1.0000 Uiso R . . . . .
H731 H 0.7679 0.1129 0.2431 0.1178 1.0000 Uiso R . . . . .
H732 H 0.7649 0.2202 0.2254 0.1183 1.0000 Uiso R . . . . .
H733 H 0.7130 0.1823 0.2892 0.1180 1.0000 Uiso R . . . . .
H741 H 0.6179 0.0698 0.1444 0.0944 1.0000 Uiso R . . . . .
H742 H 0.5668 0.0358 0.2095 0.0943 1.0000 Uiso R . . . . .
H761 H 0.4111 0.0454 0.1935 0.1172 0.48(3) Uiso R . P 1 1 .
H762 H 0.3868 0.1504 0.1864 0.1171 0.48(3) Uiso R . P 1 1 .
H771 H 0.3104 0.0162 0.0737 0.1659 0.48(3) Uiso R . P 1 1 .
H772 H 0.4289 0.0051 0.0768 0.1659 0.48(3) Uiso R . P 1 1 .
H773 H 0.4164 0.1129 0.0683 0.1663 0.48(3) Uiso R . P 1 1 .
H781 H 0.3840 0.0603 0.1650 0.1293 0.52(3) Uiso R . P 1 2 .
H782 H 0.4027 0.1799 0.1591 0.1291 0.52(3) Uiso R . P 1 2 .
H793 H 0.3487 0.0549 0.0439 0.1690 0.52(3) Uiso R . P 1 2 .
H792 H 0.4590 0.0303 0.0644 0.1690 0.52(3) Uiso R . P 1 2 .
H791 H 0.4720 0.1464 0.0577 0.1691 0.52(3) Uiso R . P 1 2 .
H801 H 0.5097 0.1823 0.3406 0.1028 1.0000 Uiso R . . . . .
H802 H 0.4121 0.2050 0.3794 0.1024 1.0000 Uiso R . . . . .
H813 H 0.5302 0.1704 0.4605 0.1231 1.0000 Uiso R . . . . .
H812 H 0.6416 0.2548 0.4474 0.1231 1.0000 Uiso R . . . . .
H811 H 0.5544 0.2945 0.4848 0.1231 1.0000 Uiso R . . . . .
H831 H 0.5443 0.4252 0.4609 0.0891 0.52(3) Uiso R . P 1 2 .
H832 H 0.4172 0.3802 0.4130 0.0891 0.52(3) Uiso R . P 1 2 .
H841 H 0.4551 0.3923 0.4370 0.1062 0.48(3) Uiso R . P 1 1 .
H842 H 0.3858 0.3687 0.3570 0.1061 0.48(3) Uiso R . P 1 1 .
H851 H 0.5100 0.5640 0.4228 0.1019 0.52(3) Uiso R . P 1 2 .
H852 H 0.6057 0.5400 0.3913 0.1019 0.52(3) Uiso R . P 1 2 .
H853 H 0.4820 0.4965 0.3439 0.1019 0.52(3) Uiso R . P 1 2 .
H854 H 0.4869 0.5558 0.4078 0.1019 0.48(3) Uiso R . P 1 1 .
H855 H 0.6009 0.5381 0.4214 0.1019 0.48(3) Uiso R . P 1 1 .
H856 H 0.5329 0.5145 0.3438 0.1019 0.48(3) Uiso R . P 1 1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          5.00(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 . Cl2 . 2.1813(16) yes
Al1 . N4 . 1.899(3) yes
Al1 . N10 . 1.896(3) yes
Al1 . C35 . 2.012(5) yes
N4 . C5 . 1.345(5) yes
N4 . C23 . 1.454(4) yes
C5 . C6 . 1.516(5) yes
C5 . C7 . 1.410(5) yes
C6 . B39 . 1.657(5) yes
C6 . H61 . 0.989 no
C6 . H62 . 0.984 no
C7 . C8 . 1.394(5) yes
C7 . H71 . 0.938 no
C8 . C9 . 1.501(5) yes
C8 . N10 . 1.352(5) yes
C9 . H91 . 0.966 no
C9 . H92 . 0.957 no
C9 . H93 . 0.962 no
N10 . C11 . 1.453(5) yes
C11 . C12 . 1.391(6) yes
C11 . C19 . 1.425(6) yes
C12 . C13 . 1.521(7) yes
C12 . C16 . 1.410(6) yes
C13 . C14 . 1.539(6) yes
C13 . C15 . 1.526(7) yes
C13 . H131 . 0.990 no
C14 . H141 . 0.971 no
C14 . H142 . 0.971 no
C14 . H143 . 0.965 no
C15 . H151 . 0.978 no
C15 . H152 . 0.975 no
C15 . H153 . 0.971 no
C16 . C17 . 1.365(8) yes
C16 . H161 . 0.939 no
C17 . C18 . 1.370(8) yes
C17 . H171 . 0.946 no
C18 . C19 . 1.399(6) yes
C18 . H181 . 0.940 no
C19 . C20 . 1.513(7) yes
C20 . C21 . 1.537(6) yes
C20 . C22 . 1.523(7) yes
C20 . H201 . 0.991 no
C21 . H211 . 0.963 no
C21 . H212 . 0.967 no
C21 . H213 . 0.967 no
C22 . H223 . 0.969 no
C22 . H222 . 0.968 no
C22 . H221 . 0.963 no
C23 . C24 . 1.408(5) yes
C23 . C31 . 1.412(5) yes
C24 . C25 . 1.526(5) yes
C24 . C28 . 1.396(5) yes
C25 . C26 . 1.536(6) yes
C25 . C27 . 1.531(6) yes
C25 . H251 . 1.003 no
C26 . H263 . 0.984 no
C26 . H262 . 0.964 no
C26 . H261 . 0.971 no
C27 . H271 . 0.965 no
C27 . H272 . 0.975 no
C27 . H273 . 0.978 no
C28 . C29 . 1.370(6) yes
C28 . H281 . 0.944 no
C29 . C30 . 1.389(6) yes
C29 . H291 . 0.950 no
C30 . C31 . 1.381(5) yes
C30 . H301 . 0.946 no
C31 . C32 . 1.522(6) yes
C32 . C33 . 1.514(6) yes
C32 . C34 . 1.538(6) yes
C32 . H321 . 0.992 no
C33 . H331 . 0.979 no
C33 . H332 . 0.984 no
C33 . H333 . 0.977 no
C34 . H341 . 0.969 no
C34 . H342 . 0.977 no
C34 . H343 . 0.975 no
C35 . C36 . 1.548(7) yes
C35 . C37 . 1.526(7) yes
C35 . C38 . 1.530(6) yes
C36 . H361 . 0.987 no
C36 . H362 . 0.980 no
C36 . H363 . 0.984 no
C37 . H373 . 1.001 no
C37 . H372 . 0.976 no
C37 . H371 . 0.967 no
C38 . H381 . 0.968 no
C38 . H382 . 0.979 no
C38 . H383 . 0.963 no
B39 . C40 . 1.654(5) yes
B39 . C51 . 1.671(5) yes
B39 . C62 . 1.659(5) yes
C40 . C41 . 1.387(5) yes
C40 . C49 . 1.397(5) yes
C41 . F42 . 1.362(5) yes
C41 . C43 . 1.380(6) yes
C43 . F44 . 1.350(5) yes
C43 . C45 . 1.373(7) yes
C45 . F46 . 1.344(5) yes
C45 . C47 . 1.378(7) yes
C47 . F48 . 1.341(5) yes
C47 . C49 . 1.387(6) yes
C49 . F50 . 1.350(5) yes
C51 . C52 . 1.386(5) yes
C51 . C60 . 1.404(5) yes
C52 . F53 . 1.356(5) yes
C52 . C54 . 1.378(6) yes
C54 . F55 . 1.355(5) yes
C54 . C56 . 1.379(6) yes
C56 . F57 . 1.339(5) yes
C56 . C58 . 1.371(6) yes
C58 . F59 . 1.350(5) yes
C58 . C60 . 1.373(5) yes
C60 . F61 . 1.360(4) yes
C62 . C63 . 1.383(6) yes
C62 . C71 . 1.389(6) yes
C63 . F64 . 1.359(5) yes
C63 . C65 . 1.384(6) yes
C65 . F66 . 1.354(6) yes
C65 . C67 . 1.354(8) yes
C67 . F68 . 1.344(5) yes
C67 . C69 . 1.372(9) yes
C69 . F70 . 1.348(6) yes
C69 . C71 . 1.386(7) yes
C71 . F72 . 1.352(6) yes
C73 . C74 . 1.479(9) yes
C73 . H731 . 0.965 no
C73 . H732 . 0.977 no
C73 . H733 . 0.975 no
C74 . O75 . 1.419(6) yes
C74 . H741 . 0.980 no
C74 . H742 . 0.989 no
O75 . C76 . 1.446(8) yes
O75 . C78 . 1.449(9) yes
C76 . C77 . 1.516(9) yes
C76 . H761 . 0.983 no
C76 . H762 . 0.993 no
C77 . H771 . 0.961 no
C77 . H772 . 0.965 no
C77 . H773 . 0.964 no
C78 . C79 . 1.509(9) yes
C78 . H781 . 0.981 no
C78 . H782 . 0.980 no
C79 . H793 . 0.968 no
C79 . H792 . 0.968 no
C79 . H791 . 0.965 no
C80 . C81 . 1.485(9) yes
C80 . O82 . 1.427(7) yes
C80 . H801 . 0.995 no
C80 . H802 . 0.994 no
C81 . H813 . 0.968 no
C81 . H812 . 0.975 no
C81 . H811 . 0.960 no
O82 . C84 . 1.425(7) yes
O82 . C83 . 1.433(7) yes
C83 . C85 . 1.486(7) yes
C83 . H831 . 0.969 no
C83 . H832 . 0.983 no
C84 . C85 . 1.494(7) yes
C84 . H841 . 0.981 no
C84 . H842 . 0.977 no
C85 . H854 . 0.950 no
C85 . H855 . 0.950 no
C85 . H856 . 0.950 no
C85 . H851 . 0.950 no
C85 . H852 . 0.950 no
C85 . H853 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 . Al1 . N4 . 103.13(11) yes
Cl2 . Al1 . N10 . 103.81(11) yes
N4 . Al1 . N10 . 98.21(14) yes
Cl2 . Al1 . C35 . 108.95(16) yes
N4 . Al1 . C35 . 121.63(16) yes
N10 . Al1 . C35 . 118.77(18) yes
Al1 . N4 . C5 . 119.2(2) yes
Al1 . N4 . C23 . 120.9(2) yes
C5 . N4 . C23 . 119.7(3) yes
N4 . C5 . C6 . 120.4(3) yes
N4 . C5 . C7 . 120.9(3) yes
C6 . C5 . C7 . 118.7(3) yes
C5 . C6 . B39 . 122.5(3) yes
C5 . C6 . H61 . 106.0 no
B39 . C6 . H61 . 107.2 no
C5 . C6 . H62 . 105.5 no
B39 . C6 . H62 . 107.1 no
H61 . C6 . H62 . 107.8 no
C5 . C7 . C8 . 129.2(3) yes
C5 . C7 . H71 . 115.2 no
C8 . C7 . H71 . 115.5 no
C7 . C8 . C9 . 116.5(3) yes
C7 . C8 . N10 . 123.2(3) yes
C9 . C8 . N10 . 120.3(3) yes
C8 . C9 . H91 . 111.7 no
C8 . C9 . H92 . 110.1 no
H91 . C9 . H92 . 108.9 no
C8 . C9 . H93 . 110.2 no
H91 . C9 . H93 . 107.6 no
H92 . C9 . H93 . 108.2 no
C8 . N10 . Al1 . 117.0(2) yes
C8 . N10 . C11 . 118.6(3) yes
Al1 . N10 . C11 . 123.8(2) yes
N10 . C11 . C12 . 121.3(4) yes
N10 . C11 . C19 . 117.4(4) yes
C12 . C11 . C19 . 121.3(4) yes
C11 . C12 . C13 . 123.3(4) yes
C11 . C12 . C16 . 118.0(4) yes
C13 . C12 . C16 . 118.7(4) yes
C12 . C13 . C14 . 110.9(4) yes
C12 . C13 . C15 . 111.4(4) yes
C14 . C13 . C15 . 109.4(4) yes
C12 . C13 . H131 . 106.6 no
C14 . C13 . H131 . 109.1 no
C15 . C13 . H131 . 109.4 no
C13 . C14 . H141 . 109.2 no
C13 . C14 . H142 . 109.1 no
H141 . C14 . H142 . 110.4 no
C13 . C14 . H143 . 108.6 no
H141 . C14 . H143 . 109.2 no
H142 . C14 . H143 . 110.3 no
C13 . C15 . H151 . 108.6 no
C13 . C15 . H152 . 109.5 no
H151 . C15 . H152 . 107.8 no
C13 . C15 . H153 . 111.1 no
H151 . C15 . H153 . 109.9 no
H152 . C15 . H153 . 110.0 no
C12 . C16 . C17 . 121.2(5) yes
C12 . C16 . H161 . 119.4 no
C17 . C16 . H161 . 119.4 no
C16 . C17 . C18 . 120.6(5) yes
C16 . C17 . H171 . 119.1 no
C18 . C17 . H171 . 120.3 no
C17 . C18 . C19 . 121.3(5) yes
C17 . C18 . H181 . 119.5 no
C19 . C18 . H181 . 119.1 no
C11 . C19 . C18 . 117.5(5) yes
C11 . C19 . C20 . 121.8(4) yes
C18 . C19 . C20 . 120.7(4) yes
C19 . C20 . C21 . 113.5(4) yes
C19 . C20 . C22 . 112.6(4) yes
C21 . C20 . C22 . 108.5(4) yes
C19 . C20 . H201 . 107.6 no
C21 . C20 . H201 . 106.4 no
C22 . C20 . H201 . 107.9 no
C20 . C21 . H211 . 109.0 no
C20 . C21 . H212 . 108.0 no
H211 . C21 . H212 . 110.6 no
C20 . C21 . H213 . 107.7 no
H211 . C21 . H213 . 111.0 no
H212 . C21 . H213 . 110.5 no
C20 . C22 . H223 . 109.5 no
C20 . C22 . H222 . 109.5 no
H223 . C22 . H222 . 110.3 no
C20 . C22 . H221 . 110.9 no
H223 . C22 . H221 . 107.9 no
H222 . C22 . H221 . 108.7 no
N4 . C23 . C24 . 121.1(3) yes
N4 . C23 . C31 . 118.0(3) yes
C24 . C23 . C31 . 120.8(3) yes
C23 . C24 . C25 . 123.9(3) yes
C23 . C24 . C28 . 118.1(4) yes
C25 . C24 . C28 . 118.0(4) yes
C24 . C25 . C26 . 111.2(4) yes
C24 . C25 . C27 . 111.9(3) yes
C26 . C25 . C27 . 109.7(4) yes
C24 . C25 . H251 . 109.0 no
C26 . C25 . H251 . 106.7 no
C27 . C25 . H251 . 108.1 no
C25 . C26 . H263 . 108.6 no
C25 . C26 . H262 . 108.1 no
H263 . C26 . H262 . 109.2 no
C25 . C26 . H261 . 108.9 no
H263 . C26 . H261 . 111.3 no
H262 . C26 . H261 . 110.7 no
C25 . C27 . H271 . 108.1 no
C25 . C27 . H272 . 111.5 no
H271 . C27 . H272 . 110.3 no
C25 . C27 . H273 . 108.9 no
H271 . C27 . H273 . 109.0 no
H272 . C27 . H273 . 109.0 no
C24 . C28 . C29 . 121.5(4) yes
C24 . C28 . H281 . 118.5 no
C29 . C28 . H281 . 119.9 no
C28 . C29 . C30 . 119.8(4) yes
C28 . C29 . H291 . 120.4 no
C30 . C29 . H291 . 119.8 no
C29 . C30 . C31 . 121.4(4) yes
C29 . C30 . H301 . 119.5 no
C31 . C30 . H301 . 119.2 no
C23 . C31 . C30 . 118.3(4) yes
C23 . C31 . C32 . 121.9(3) yes
C30 . C31 . C32 . 119.7(3) yes
C31 . C32 . C33 . 112.0(4) yes
C31 . C32 . C34 . 113.1(4) yes
C33 . C32 . C34 . 110.4(4) yes
C31 . C32 . H321 . 107.0 no
C33 . C32 . H321 . 107.1 no
C34 . C32 . H321 . 106.8 no
C32 . C33 . H331 . 110.4 no
C32 . C33 . H332 . 107.1 no
H331 . C33 . H332 . 110.2 no
C32 . C33 . H333 . 108.6 no
H331 . C33 . H333 . 109.4 no
H332 . C33 . H333 . 111.0 no
C32 . C34 . H341 . 108.4 no
C32 . C34 . H342 . 108.7 no
H341 . C34 . H342 . 110.9 no
C32 . C34 . H343 . 109.7 no
H341 . C34 . H343 . 109.1 no
H342 . C34 . H343 . 110.0 no
Al1 . C35 . C36 . 114.6(3) yes
Al1 . C35 . C37 . 108.7(3) yes
C36 . C35 . C37 . 105.9(5) yes
Al1 . C35 . C38 . 111.1(3) yes
C36 . C35 . C38 . 107.5(4) yes
C37 . C35 . C38 . 108.7(4) yes
C35 . C36 . H361 . 109.4 no
C35 . C36 . H362 . 109.1 no
H361 . C36 . H362 . 110.3 no
C35 . C36 . H363 . 108.1 no
H361 . C36 . H363 . 110.5 no
H362 . C36 . H363 . 109.4 no
C35 . C37 . H373 . 106.1 no
C35 . C37 . H372 . 108.8 no
H373 . C37 . H372 . 111.1 no
C35 . C37 . H371 . 109.1 no
H373 . C37 . H371 . 110.6 no
H372 . C37 . H371 . 110.9 no
C35 . C38 . H381 . 110.0 no
C35 . C38 . H382 . 108.6 no
H381 . C38 . H382 . 109.9 no
C35 . C38 . H383 . 109.0 no
H381 . C38 . H383 . 109.7 no
H382 . C38 . H383 . 109.6 no
C6 . B39 . C40 . 105.3(3) yes
C6 . B39 . C51 . 107.9(3) yes
C40 . B39 . C51 . 112.7(3) yes
C6 . B39 . C62 . 116.2(3) yes
C40 . B39 . C62 . 113.1(3) yes
C51 . B39 . C62 . 101.7(3) yes
B39 . C40 . C41 . 127.3(3) yes
B39 . C40 . C49 . 119.5(3) yes
C41 . C40 . C49 . 112.6(3) yes
C40 . C41 . F42 . 120.6(3) yes
C40 . C41 . C43 . 124.9(4) yes
F42 . C41 . C43 . 114.5(4) yes
C41 . C43 . F44 . 121.1(4) yes
C41 . C43 . C45 . 119.6(4) yes
F44 . C43 . C45 . 119.3(4) yes
C43 . C45 . F46 . 121.2(4) yes
C43 . C45 . C47 . 119.1(4) yes
F46 . C45 . C47 . 119.7(5) yes
C45 . C47 . F48 . 120.1(4) yes
C45 . C47 . C49 . 119.0(4) yes
F48 . C47 . C49 . 120.9(4) yes
C40 . C49 . C47 . 124.8(4) yes
C40 . C49 . F50 . 119.9(3) yes
C47 . C49 . F50 . 115.3(4) yes
B39 . C51 . C52 . 128.8(3) yes
B39 . C51 . C60 . 119.3(3) yes
C52 . C51 . C60 . 111.8(3) yes
C51 . C52 . F53 . 120.5(3) yes
C51 . C52 . C54 . 124.6(4) yes
F53 . C52 . C54 . 114.8(4) yes
C52 . C54 . F55 . 120.8(4) yes
C52 . C54 . C56 . 120.3(4) yes
F55 . C54 . C56 . 118.9(4) yes
C54 . C56 . F57 . 121.0(4) yes
C54 . C56 . C58 . 118.2(4) yes
F57 . C56 . C58 . 120.8(4) yes
C56 . C58 . F59 . 120.0(4) yes
C56 . C58 . C60 . 119.4(4) yes
F59 . C58 . C60 . 120.6(4) yes
C51 . C60 . C58 . 125.4(4) yes
C51 . C60 . F61 . 119.3(3) yes
C58 . C60 . F61 . 115.2(3) yes
B39 . C62 . C63 . 127.4(4) yes
B39 . C62 . C71 . 119.7(4) yes
C63 . C62 . C71 . 112.6(4) yes
C62 . C63 . F64 . 120.6(3) yes
C62 . C63 . C65 . 124.4(5) yes
F64 . C63 . C65 . 115.0(4) yes
C63 . C65 . F66 . 119.6(5) yes
C63 . C65 . C67 . 120.2(5) yes
F66 . C65 . C67 . 120.3(4) yes
C65 . C67 . F68 . 121.3(6) yes
C65 . C67 . C69 . 118.8(4) yes
F68 . C67 . C69 . 119.8(6) yes
C67 . C69 . F70 . 119.9(5) yes
C67 . C69 . C71 . 119.3(5) yes
F70 . C69 . C71 . 120.7(6) yes
C62 . C71 . C69 . 124.6(5) yes
C62 . C71 . F72 . 119.4(4) yes
C69 . C71 . F72 . 116.0(4) yes
C74 . C73 . H731 . 111.4 no
C74 . C73 . H732 . 108.5 no
H731 . C73 . H732 . 109.8 no
C74 . C73 . H733 . 107.5 no
H731 . C73 . H733 . 109.3 no
H732 . C73 . H733 . 110.4 no
C73 . C74 . O75 . 109.1(5) yes
C73 . C74 . H741 . 109.5 no
O75 . C74 . H741 . 109.1 no
C73 . C74 . H742 . 109.0 no
O75 . C74 . H742 . 111.0 no
H741 . C74 . H742 . 109.1 no
C74 . O75 . C76 . 108.4(11) yes
C74 . O75 . C78 . 117.8(10) yes
O75 . C76 . C77 . 108.64(10) yes
O75 . C76 . H761 . 110.3 no
C77 . C76 . H761 . 108.3 no
O75 . C76 . H762 . 110.0 no
C77 . C76 . H762 . 111.5 no
H761 . C76 . H762 . 108.0 no
C76 . C77 . H771 . 111.9 no
C76 . C77 . H772 . 109.5 no
H771 . C77 . H772 . 109.0 no
C76 . C77 . H773 . 107.3 no
H771 . C77 . H773 . 109.3 no
H772 . C77 . H773 . 109.7 no
O75 . C78 . C79 . 108.64(10) yes
O75 . C78 . H781 . 113.5 no
C79 . C78 . H781 . 108.7 no
O75 . C78 . H782 . 107.0 no
C79 . C78 . H782 . 109.3 no
H781 . C78 . H782 . 109.6 no
C78 . C79 . H793 . 111.1 no
C78 . C79 . H792 . 109.1 no
H793 . C79 . H792 . 108.9 no
C78 . C79 . H791 . 108.8 no
H793 . C79 . H791 . 109.8 no
H792 . C79 . H791 . 109.1 no
C81 . C80 . O82 . 112.5(5) yes
C81 . C80 . H801 . 109.3 no
O82 . C80 . H801 . 107.3 no
C81 . C80 . H802 . 108.4 no
O82 . C80 . H802 . 108.5 no
H801 . C80 . H802 . 110.9 no
C80 . C81 . H813 . 109.3 no
C80 . C81 . H812 . 109.1 no
H813 . C81 . H812 . 109.8 no
C80 . C81 . H811 . 107.5 no
H813 . C81 . H811 . 109.0 no
H812 . C81 . H811 . 111.9 no
C80 . O82 . C84 . 114.7(6) yes
C80 . O82 . C83 . 112.1(4) yes
O82 . C83 . C85 . 108.58(10) yes
O82 . C83 . H831 . 109.4 no
C85 . C83 . H831 . 110.1 no
O82 . C83 . H832 . 110.0 no
C85 . C83 . H832 . 109.8 no
H831 . C83 . H832 . 108.9 no
O82 . C84 . C85 . 108.57(10) yes
O82 . C84 . H841 . 109.1 no
C85 . C84 . H841 . 109.5 no
O82 . C84 . H842 . 110.4 no
C85 . C84 . H842 . 110.2 no
H841 . C84 . H842 . 109.2 no
C84 . C85 . H854 . 110.6 no
C84 . C85 . H855 . 109.5 no
H854 . C85 . H855 . 109.5 no
C84 . C85 . H856 . 108.3 no
H854 . C85 . H856 . 109.5 no
H855 . C85 . H856 . 109.5 no
C83 . C85 . H851 . 110.3 no
C83 . C85 . H852 . 108.7 no
H851 . C85 . H852 . 109.5 no
C83 . C85 . H853 . 109.4 no
H851 . C85 . H853 . 109.5 no
H852 . C85 . H853 . 109.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C7 . H71 . C62 . 139.44 0.938 2.585 3.354(9) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 11/11/13 at 16:00:12
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 223,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 263,X'S) H   ( 262,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 373,X'S) H   ( 372,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) H   ( 733,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) H   ( 773,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 793,X'S) H   ( 792,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) H   ( 802,X'S) 
RIDE C   (  81,X'S) H   ( 813,X'S) H   ( 812,X'S) H   ( 811,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 832,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C(85,X'S) H(854,X'S) H(855,X'S) H(856,X'S) H(851,X'S) H(852,X'S) H(853,X'S)
 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 11/11/13 at 16:00:12
#
#LIST     16                                                                    
REM 
REM ET2O DISORDER 
REM 
SAME  O(75)  C(78)  C(79) AND 
CONT  O(75)  C(76)  C(77) AND 
CONT  O(82)  C(83)  C(85) AND 
CONT  O(82)  C(84)  C(85) 
SIMU 0.01 O(75)  C(78)  C(79) AND 
CONT  O(75)  C(76)  C(77) AND 
CONT  O(82)  C(83)  C(85) AND 
CONT  O(82)  C(84)  C(85) 
DELU 0.01 O(75)  C(78)  C(79) AND 
CONT  O(75)  C(76)  C(77) AND 
CONT  O(82)  C(83)  C(85) AND 
CONT  O(82)  C(84)  C(85) 
END                                                                             
;

# start Validation Reply Form
_vrf_DIFMX01_132JART13           
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: Due to the lamellar structure of the crystal, 
the
residual density is attributed to a twinning impurity that 
cannot be model through the usual twinning laws.
;
_vrf_PLAT097_132JART13           
;
PROBLEM: Large Reported Max. (Positive) Residual Density  1.98 eA-3  
RESPONSE: confer DIFMX01
;
# end Validation Reply Form
####################################################################### 
# 
# 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_154JART14
_database_code_depnum_ccdc_archive 'CCDC 1544789'
_audit_update_record             
;
2017-04-18 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_audit_creation_date             2014-01-26
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '154JART14 in P n a 21'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   18.4434(2)
_cell_length_b                   17.7597(2)
_cell_length_c                   17.6898(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5794.28(11)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21 '
_symmetry_space_group_name_Hall  'P 2c -2n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z+1/2
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C57 H60 B1 F15 N2 O1 
# Dc =      1.24 Fooo =   2256.00 Mu =      9.20 M =   1084.90
# Found Formula = C57 H55 B2 F15 N2 O1 
# Dc =      1.25 FOOO =   2256.00 Mu =      9.23 M =   1090.67

_chemical_formula_sum            'C57 H55 B2 F15 N2 O1'
_chemical_formula_moiety         'C57 H55 B2 F15 N2 O1'
_chemical_compound_source        ?
_chemical_formula_weight         1090.67


_cell_measurement_reflns_used    19434
_cell_measurement_theta_min      3
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.160
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_max          0.260

_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2256
_exptl_absorpt_coefficient_mu    0.923

# Sheldrick geometric approximatio 0.82 0.86 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.86
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            10536
_reflns_number_total             10536
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 10536 
# Number of reflections with Friedels Law is 6249 
# Theoretical number of reflections is about 6072 


_diffrn_reflns_theta_min         3.455
_diffrn_reflns_theta_max         76.289
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        74.763
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              0
_reflns_limit_h_max              23
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              -17
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   2.77
_oxford_diffrn_Wilson_scale      0.09

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.15
_refine_diff_density_max         0.17


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         10500
_refine_ls_number_restraints     1
_refine_ls_number_parameters     694
_oxford_refine_ls_R_factor_ref   0.0314
_refine_ls_wR_factor_ref         0.0807
_refine_ls_goodness_of_fit_ref   0.9867
_refine_ls_shift/su_max          0.0014948
_refine_ls_shift/su_mean         0.0001456


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10500
_refine_ls_R_factor_all          0.0314
_refine_ls_wR_factor_all         0.0807

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10079
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_gt          0.0784

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration unk


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 0.70P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.30089(5) 0.61342(5) 0.26355(6) 0.0308 1.0000 Uani . . . . . .
C2 C 0.28568(8) 0.55053(8) 0.22320(9) 0.0251 1.0000 Uani . . . . . .
C3 C 0.30198(9) 0.55443(8) 0.14729(9) 0.0293 1.0000 Uani . . . . . .
F4 F 0.33234(6) 0.61631(6) 0.11723(6) 0.0425 1.0000 Uani . . . . . .
C5 C 0.28525(9) 0.49433(10) 0.10089(9) 0.0325 1.0000 Uani . . . . . .
F6 F 0.29762(6) 0.49788(7) 0.02627(6) 0.0448 1.0000 Uani . . . . . .
C7 C 0.25344(9) 0.43161(9) 0.13232(9) 0.0316 1.0000 Uani . . . . . .
F8 F 0.23613(7) 0.37327(6) 0.08743(7) 0.0446 1.0000 Uani . . . . . .
C9 C 0.23873(9) 0.43002(8) 0.20912(9) 0.0280 1.0000 Uani . . . . . .
C10 C 0.25348(8) 0.48906(8) 0.25874(8) 0.0236 1.0000 Uani . . . . . .
B11 B 0.22718(8) 0.49583(8) 0.34822(9) 0.0213 1.0000 Uani . . . . . .
C12 C 0.29726(7) 0.52263(7) 0.40121(8) 0.0204 1.0000 Uani . . . . . .
C13 C 0.28731(7) 0.51846(7) 0.48526(8) 0.0196 1.0000 Uani . . . . . .
N14 N 0.34581(6) 0.51262(6) 0.53197(7) 0.0191 1.0000 Uani . . . . . .
C15 C 0.41692(7) 0.53112(7) 0.50134(8) 0.0208 1.0000 Uani . . . . . .
C16 C 0.46817(8) 0.47402(8) 0.48803(8) 0.0248 1.0000 Uani . . . . . .
C17 C 0.53823(8) 0.49669(9) 0.46791(10) 0.0321 1.0000 Uani . . . . . .
C18 C 0.55598(9) 0.57221(10) 0.46029(10) 0.0358 1.0000 Uani . . . . . .
C19 C 0.50353(9) 0.62687(9) 0.47128(10) 0.0321 1.0000 Uani . . . . . .
C20 C 0.43272(8) 0.60807(8) 0.49208(9) 0.0255 1.0000 Uani . . . . . .
C21 C 0.37797(9) 0.67069(8) 0.50555(10) 0.0303 1.0000 Uani . . . . . .
C22 C 0.37554(11) 0.72651(9) 0.43931(12) 0.0429 1.0000 Uani . . . . . .
C23 C 0.39244(11) 0.71227(9) 0.58002(12) 0.0417 1.0000 Uani . . . . . .
C24 C 0.45097(8) 0.39052(8) 0.49282(10) 0.0307 1.0000 Uani . . . . . .
C25 C 0.49352(12) 0.35163(10) 0.55599(12) 0.0443 1.0000 Uani . . . . . .
C26 C 0.46760(10) 0.35157(10) 0.41736(11) 0.0393 1.0000 Uani . . . . . .
B27 B 0.33901(8) 0.49631(8) 0.61238(9) 0.0204 1.0000 Uani . . . . . .
N28 N 0.26460(6) 0.49056(6) 0.63945(7) 0.0215 1.0000 Uani . . . . . .
C29 C 0.20722(7) 0.50759(7) 0.59418(8) 0.0225 1.0000 Uani . . . . . .
C30 C 0.21886(7) 0.52004(7) 0.51801(8) 0.0218 1.0000 Uani . . . . . .
C31 C 0.13186(8) 0.51145(9) 0.62557(9) 0.0313 1.0000 Uani . . . . . .
C32 C 0.24934(8) 0.46856(8) 0.71722(9) 0.0262 1.0000 Uani . . . . . .
C33 C 0.26134(9) 0.52078(9) 0.77474(9) 0.0318 1.0000 Uani . . . . . .
C34 C 0.28597(10) 0.60068(9) 0.75933(10) 0.0358 1.0000 Uani . . . . . .
C35 C 0.34813(11) 0.62480(11) 0.81113(12) 0.0455 1.0000 Uani . . . . . .
C36 C 0.22188(13) 0.65532(12) 0.76563(16) 0.0582 1.0000 Uani . . . . . .
C37 C 0.24847(12) 0.49672(12) 0.84877(11) 0.0466 1.0000 Uani . . . . . .
C38 C 0.22640(15) 0.42341(15) 0.86381(11) 0.0597 1.0000 Uani . . . . . .
C40 C 0.21479(13) 0.37362(12) 0.80519(11) 0.0486 1.0000 Uani . . . . . .
C41 C 0.22548(9) 0.39465(9) 0.73051(10) 0.0337 1.0000 Uani . . . . . .
C43 C 0.21223(10) 0.33754(9) 0.66717(11) 0.0371 1.0000 Uani . . . . . .
C42 C 0.13966(10) 0.29719(11) 0.67537(13) 0.0456 1.0000 Uani . . . . . .
C44 C 0.27291(13) 0.27919(15) 0.6609(2) 0.0693 1.0000 Uani . . . . . .
C45 C 0.40592(8) 0.48584(7) 0.66706(8) 0.0232 1.0000 Uani . . . . . .
C46 C 0.46634(8) 0.53370(8) 0.66595(9) 0.0259 1.0000 Uani . . . . . .
C47 C 0.52463(9) 0.52325(9) 0.71457(10) 0.0324 1.0000 Uani . . . . . .
C48 C 0.52488(9) 0.46365(9) 0.76519(10) 0.0347 1.0000 Uani . . . . . .
C49 C 0.46630(9) 0.41464(9) 0.76708(10) 0.0334 1.0000 Uani . . . . . .
C52 C 0.40735(8) 0.42637(8) 0.71939(9) 0.0282 1.0000 Uani . . . . . .
C50 C 0.16075(8) 0.55861(8) 0.34106(8) 0.0244 1.0000 Uani . . . . . .
C51 C 0.16266(8) 0.63317(8) 0.36439(9) 0.0273 1.0000 Uani . . . . . .
F52 F 0.21939(5) 0.66046(5) 0.40451(6) 0.0330 1.0000 Uani . . . . . .
C53 C 0.10956(9) 0.68585(9) 0.34819(11) 0.0356 1.0000 Uani . . . . . .
F54 F 0.11658(7) 0.75797(5) 0.37073(7) 0.0474 1.0000 Uani . . . . . .
C55 C 0.04924(11) 0.66450(11) 0.30810(13) 0.0465 1.0000 Uani . . . . . .
F56 F -0.00332(8) 0.71464(7) 0.29303(11) 0.0717 1.0000 Uani . . . . . .
C57 C 0.04364(10) 0.59052(11) 0.28420(13) 0.0454 1.0000 Uani . . . . . .
C58 C 0.09882(9) 0.54088(9) 0.29967(10) 0.0330 1.0000 Uani . . . . . .
F59 F 0.09117(6) 0.47072(5) 0.27186(7) 0.0408 1.0000 Uani . . . . . .
F60 F -0.01520(8) 0.56839(7) 0.24496(11) 0.0730 1.0000 Uani . . . . . .
C61 C 0.20192(8) 0.41385(7) 0.38330(8) 0.0240 1.0000 Uani . . . . . .
C62 C 0.25200(8) 0.35494(8) 0.38546(9) 0.0272 1.0000 Uani . . . . . .
F63 F 0.31577(5) 0.36252(5) 0.34819(6) 0.0347 1.0000 Uani . . . . . .
C64 C 0.24166(11) 0.28795(9) 0.42332(10) 0.0355 1.0000 Uani . . . . . .
F65 F 0.29440(8) 0.23582(6) 0.42583(7) 0.0490 1.0000 Uani . . . . . .
C66 C 0.17654(12) 0.27447(9) 0.45910(10) 0.0388 1.0000 Uani . . . . . .
F67 F 0.16525(8) 0.20852(6) 0.49413(7) 0.0538 1.0000 Uani . . . . . .
C68 C 0.12423(10) 0.32909(9) 0.45761(10) 0.0374 1.0000 Uani . . . . . .
C69 C 0.13784(9) 0.39674(8) 0.42139(9) 0.0299 1.0000 Uani . . . . . .
F70 F 0.08425(5) 0.44826(6) 0.42699(7) 0.0389 1.0000 Uani . . . . . .
F71 F 0.06046(7) 0.31748(7) 0.49198(8) 0.0537 1.0000 Uani . . . . . .
F72 F 0.20604(6) 0.36614(5) 0.23317(6) 0.0376 1.0000 Uani . . . . . .
O73 O 0.42901(7) 0.21590(7) 0.16330(8) 0.0415 1.0000 Uani . . . . . .
C74 C 0.38388(11) 0.26875(10) 0.12613(12) 0.0423 1.0000 Uani . . . . . .
C75 C 0.35051(15) 0.23102(14) 0.05855(14) 0.0609 1.0000 Uani . . . . . .
C76 C 0.45749(11) 0.24544(10) 0.23173(13) 0.0455 1.0000 Uani . . . . . .
C77 C 0.50543(16) 0.18665(15) 0.26667(19) 0.0705 1.0000 Uani . . . . . .
H121 H 0.3059 0.5750 0.3894 0.0243 1.0000 Uiso R . . . . .
H122 H 0.3397 0.4920 0.3869 0.0250 1.0000 Uiso R . . . . .
H171 H 0.5733 0.4596 0.4599 0.0358 1.0000 Uiso R . . . . .
H181 H 0.6054 0.5867 0.4465 0.0431 1.0000 Uiso R . . . . .
H191 H 0.5157 0.6777 0.4662 0.0408 1.0000 Uiso R . . . . .
H211 H 0.3299 0.6468 0.5103 0.0353 1.0000 Uiso R . . . . .
H221 H 0.3358 0.7602 0.4461 0.0636 1.0000 Uiso R . . . . .
H222 H 0.4209 0.7528 0.4365 0.0638 1.0000 Uiso R . . . . .
H223 H 0.3677 0.6976 0.3945 0.0642 1.0000 Uiso R . . . . .
H231 H 0.3519 0.7450 0.5877 0.0660 1.0000 Uiso R . . . . .
H232 H 0.4375 0.7395 0.5749 0.0658 1.0000 Uiso R . . . . .
H233 H 0.3943 0.6747 0.6195 0.0663 1.0000 Uiso R . . . . .
H241 H 0.3999 0.3852 0.5049 0.0362 1.0000 Uiso R . . . . .
H251 H 0.4739 0.3022 0.5600 0.0626 1.0000 Uiso R . . . . .
H252 H 0.4867 0.3789 0.6021 0.0630 1.0000 Uiso R . . . . .
H253 H 0.5431 0.3501 0.5412 0.0627 1.0000 Uiso R . . . . .
H261 H 0.4443 0.3026 0.4190 0.0607 1.0000 Uiso R . . . . .
H262 H 0.5199 0.3467 0.4118 0.0612 1.0000 Uiso R . . . . .
H263 H 0.4466 0.3804 0.3774 0.0612 1.0000 Uiso R . . . . .
H301 H 0.1782 0.5261 0.4867 0.0270 1.0000 Uiso R . . . . .
H311 H 0.1009 0.4946 0.5866 0.0460 1.0000 Uiso R . . . . .
H313 H 0.1187 0.5612 0.6410 0.0465 1.0000 Uiso R . . . . .
H312 H 0.1287 0.4765 0.6676 0.0460 1.0000 Uiso R . . . . .
H341 H 0.3048 0.6022 0.7069 0.0429 1.0000 Uiso R . . . . .
H352 H 0.3679 0.6726 0.7942 0.0700 1.0000 Uiso R . . . . .
H351 H 0.3302 0.6301 0.8607 0.0700 1.0000 Uiso R . . . . .
H353 H 0.3867 0.5872 0.8113 0.0696 1.0000 Uiso R . . . . .
H361 H 0.2408 0.7047 0.7530 0.0942 1.0000 Uiso R . . . . .
H362 H 0.2019 0.6540 0.8170 0.0941 1.0000 Uiso R . . . . .
H363 H 0.1846 0.6405 0.7299 0.0942 1.0000 Uiso R . . . . .
H371 H 0.2561 0.5293 0.8876 0.0571 1.0000 Uiso R . . . . .
H381 H 0.2191 0.4085 0.9123 0.0730 1.0000 Uiso R . . . . .
H401 H 0.1994 0.3248 0.8163 0.0582 1.0000 Uiso R . . . . .
H431 H 0.2086 0.3661 0.6187 0.0451 1.0000 Uiso R . . . . .
H421 H 0.1335 0.2667 0.6315 0.0696 1.0000 Uiso R . . . . .
H423 H 0.1413 0.2673 0.7194 0.0696 1.0000 Uiso R . . . . .
H422 H 0.1029 0.3347 0.6784 0.0697 1.0000 Uiso R . . . . .
H441 H 0.2641 0.2471 0.6180 0.1141 1.0000 Uiso R . . . . .
H443 H 0.2674 0.2493 0.7073 0.1142 1.0000 Uiso R . . . . .
H442 H 0.3203 0.3015 0.6594 0.1139 1.0000 Uiso R . . . . .
H461 H 0.4652 0.5749 0.6340 0.0300 1.0000 Uiso R . . . . .
H471 H 0.5651 0.5552 0.7112 0.0389 1.0000 Uiso R . . . . .
H481 H 0.5641 0.4572 0.7969 0.0395 1.0000 Uiso R . . . . .
H491 H 0.4652 0.3736 0.7988 0.0413 1.0000 Uiso R . . . . .
H521 H 0.3689 0.3936 0.7228 0.0333 1.0000 Uiso R . . . . .
H742 H 0.4092 0.3141 0.1114 0.0498 1.0000 Uiso R . . . . .
H741 H 0.3446 0.2860 0.1603 0.0493 1.0000 Uiso R . . . . .
H751 H 0.3277 0.2717 0.0294 0.0970 1.0000 Uiso R . . . . .
H753 H 0.3890 0.2080 0.0301 0.0968 1.0000 Uiso R . . . . .
H752 H 0.3152 0.1959 0.0755 0.0969 1.0000 Uiso R . . . . .
H761 H 0.4854 0.2908 0.2203 0.0579 1.0000 Uiso R . . . . .
H762 H 0.4176 0.2575 0.2671 0.0583 1.0000 Uiso R . . . . .
H771 H 0.5453 0.2059 0.2965 0.1100 1.0000 Uiso R . . . . .
H772 H 0.5261 0.1583 0.2246 0.1100 1.0000 Uiso R . . . . .
H773 H 0.4781 0.1521 0.2957 0.1101 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.27(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
F1 . C2 . 1.3549(17) yes
C2 . C3 . 1.378(2) yes
C2 . C10 . 1.393(2) yes
C3 . F4 . 1.3430(18) yes
C3 . C5 . 1.381(2) yes
C5 . F6 . 1.3411(19) yes
C5 . C7 . 1.376(2) yes
C7 . F8 . 1.3438(18) yes
C7 . C9 . 1.386(2) yes
C9 . C10 . 1.394(2) yes
C9 . F72 . 1.3534(18) yes
C10 . B11 . 1.660(2) yes
B11 . C12 . 1.6661(19) yes
B11 . C50 . 1.661(2) yes
B11 . C61 . 1.6499(19) yes
C12 . C13 . 1.5000(18) yes
C12 . H121 . 0.967 no
C12 . H122 . 0.986 no
C13 . N14 . 1.3629(17) yes
C13 . C30 . 1.3894(18) yes
N14 . C15 . 1.4567(17) yes
N14 . B27 . 1.4570(19) yes
C15 . C16 . 1.4061(19) yes
C15 . C20 . 1.4068(18) yes
C16 . C17 . 1.399(2) yes
C16 . C24 . 1.5188(19) yes
C17 . C18 . 1.387(2) yes
C17 . H171 . 0.934 no
C18 . C19 . 1.384(3) yes
C18 . H181 . 0.978 no
C19 . C20 . 1.397(2) yes
C19 . H191 . 0.934 no
C20 . C21 . 1.521(2) yes
C21 . C22 . 1.536(2) yes
C21 . C23 . 1.534(2) yes
C21 . H211 . 0.986 no
C22 . H221 . 0.953 no
C22 . H222 . 0.959 no
C22 . H223 . 0.955 no
C23 . H231 . 0.956 no
C23 . H232 . 0.965 no
C23 . H233 . 0.967 no
C24 . C25 . 1.530(3) yes
C24 . C26 . 1.535(2) yes
C24 . H241 . 0.971 no
C25 . H251 . 0.953 no
C25 . H252 . 0.957 no
C25 . H253 . 0.952 no
C26 . H261 . 0.970 no
C26 . H262 . 0.974 no
C26 . H263 . 0.955 no
B27 . N28 . 1.4571(19) yes
B27 . C45 . 1.579(2) yes
N28 . C29 . 1.3613(18) yes
N28 . C32 . 1.4575(18) yes
C29 . C30 . 1.382(2) yes
C29 . C31 . 1.4983(19) yes
C30 . H301 . 0.939 no
C31 . H311 . 0.943 no
C31 . H313 . 0.956 no
C31 . H312 . 0.970 no
C32 . C33 . 1.394(2) yes
C32 . C41 . 1.404(2) yes
C33 . C34 . 1.515(2) yes
C33 . C37 . 1.398(2) yes
C34 . C35 . 1.529(2) yes
C34 . C36 . 1.533(3) yes
C34 . H341 . 0.991 no
C35 . H352 . 0.971 no
C35 . H351 . 0.941 no
C35 . H353 . 0.975 no
C36 . H361 . 0.969 no
C36 . H362 . 0.981 no
C36 . H363 . 0.971 no
C37 . C38 . 1.390(3) yes
C37 . H371 . 0.908 no
C38 . C40 . 1.379(3) yes
C38 . H381 . 0.907 no
C40 . C41 . 1.387(2) yes
C40 . H401 . 0.933 no
C41 . C43 . 1.531(2) yes
C43 . C42 . 1.525(2) yes
C43 . C44 . 1.529(3) yes
C43 . H431 . 0.999 no
C42 . H421 . 0.954 no
C42 . H423 . 0.943 no
C42 . H422 . 0.951 no
C44 . H441 . 0.963 no
C44 . H443 . 0.983 no
C44 . H442 . 0.960 no
C45 . C46 . 1.402(2) yes
C45 . C52 . 1.405(2) yes
C46 . C47 . 1.389(2) yes
C46 . H461 . 0.924 no
C47 . C48 . 1.386(2) yes
C47 . H471 . 0.939 no
C48 . C49 . 1.388(2) yes
C48 . H481 . 0.923 no
C49 . C52 . 1.392(2) yes
C49 . H491 . 0.920 no
C52 . H521 . 0.919 no
C50 . C51 . 1.387(2) yes
C50 . C58 . 1.393(2) yes
C51 . F52 . 1.3542(17) yes
C51 . C53 . 1.384(2) yes
C53 . F54 . 1.3475(18) yes
C53 . C55 . 1.373(3) yes
C55 . F56 . 1.343(2) yes
C55 . C57 . 1.384(3) yes
C57 . C58 . 1.374(2) yes
C57 . F60 . 1.347(2) yes
C58 . F59 . 1.3470(19) yes
C61 . C62 . 1.396(2) yes
C61 . C69 . 1.394(2) yes
C62 . F63 . 1.3550(19) yes
C62 . C64 . 1.379(2) yes
C64 . F65 . 1.344(2) yes
C64 . C66 . 1.378(3) yes
C66 . F67 . 1.3414(18) yes
C66 . C68 . 1.368(3) yes
C68 . C69 . 1.385(2) yes
C68 . F71 . 1.340(2) yes
C69 . F70 . 1.3506(19) yes
O73 . C74 . 1.416(2) yes
O73 . C76 . 1.420(3) yes
C74 . C75 . 1.502(3) yes
C74 . H742 . 0.966 no
C74 . H741 . 0.992 no
C75 . H751 . 0.983 no
C75 . H753 . 0.962 no
C75 . H752 . 0.950 no
C76 . C77 . 1.501(3) yes
C76 . H761 . 0.977 no
C76 . H762 . 0.990 no
C77 . H771 . 0.969 no
C77 . H772 . 0.977 no
C77 . H773 . 0.946 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F1 . C2 . C3 . 115.26(13) yes
F1 . C2 . C10 . 119.78(13) yes
C3 . C2 . C10 . 124.92(14) yes
C2 . C3 . F4 . 121.21(14) yes
C2 . C3 . C5 . 119.44(14) yes
F4 . C3 . C5 . 119.34(14) yes
C3 . C5 . F6 . 120.70(15) yes
C3 . C5 . C7 . 118.72(15) yes
F6 . C5 . C7 . 120.55(15) yes
C5 . C7 . F8 . 119.11(15) yes
C5 . C7 . C9 . 119.74(14) yes
F8 . C7 . C9 . 121.14(15) yes
C7 . C9 . C10 . 124.31(14) yes
C7 . C9 . F72 . 114.36(13) yes
C10 . C9 . F72 . 121.30(14) yes
C9 . C10 . C2 . 112.86(14) yes
C9 . C10 . B11 . 126.71(13) yes
C2 . C10 . B11 . 119.89(12) yes
C10 . B11 . C12 . 109.30(11) yes
C10 . B11 . C50 . 101.04(11) yes
C12 . B11 . C50 . 115.04(11) yes
C10 . B11 . C61 . 112.17(11) yes
C12 . B11 . C61 . 105.04(11) yes
C50 . B11 . C61 . 114.37(11) yes
B11 . C12 . C13 . 116.66(11) yes
B11 . C12 . H121 . 106.3 no
C13 . C12 . H121 . 106.4 no
B11 . C12 . H122 . 108.3 no
C13 . C12 . H122 . 109.0 no
H121 . C12 . H122 . 110.1 no
C12 . C13 . N14 . 120.53(12) yes
C12 . C13 . C30 . 121.56(12) yes
N14 . C13 . C30 . 117.91(12) yes
C13 . N14 . C15 . 118.04(11) yes
C13 . N14 . B27 . 122.61(12) yes
C15 . N14 . B27 . 119.04(11) yes
N14 . C15 . C16 . 120.32(11) yes
N14 . C15 . C20 . 116.67(12) yes
C16 . C15 . C20 . 122.81(13) yes
C15 . C16 . C17 . 117.11(13) yes
C15 . C16 . C24 . 123.67(12) yes
C17 . C16 . C24 . 119.20(13) yes
C16 . C17 . C18 . 121.38(15) yes
C16 . C17 . H171 . 118.3 no
C18 . C17 . H171 . 120.3 no
C17 . C18 . C19 . 119.98(14) yes
C17 . C18 . H181 . 119.9 no
C19 . C18 . H181 . 120.2 no
C18 . C19 . C20 . 121.50(14) yes
C18 . C19 . H191 . 119.7 no
C20 . C19 . H191 . 118.8 no
C15 . C20 . C19 . 117.15(13) yes
C15 . C20 . C21 . 123.68(13) yes
C19 . C20 . C21 . 119.15(13) yes
C20 . C21 . C22 . 111.83(15) yes
C20 . C21 . C23 . 111.78(13) yes
C22 . C21 . C23 . 110.47(13) yes
C20 . C21 . H211 . 107.2 no
C22 . C21 . H211 . 108.4 no
C23 . C21 . H211 . 106.9 no
C21 . C22 . H221 . 109.3 no
C21 . C22 . H222 . 109.2 no
H221 . C22 . H222 . 111.8 no
C21 . C22 . H223 . 106.9 no
H221 . C22 . H223 . 108.9 no
H222 . C22 . H223 . 110.5 no
C21 . C23 . H231 . 106.2 no
C21 . C23 . H232 . 108.1 no
H231 . C23 . H232 . 112.5 no
C21 . C23 . H233 . 107.1 no
H231 . C23 . H233 . 110.2 no
H232 . C23 . H233 . 112.5 no
C16 . C24 . C25 . 111.99(14) yes
C16 . C24 . C26 . 110.48(14) yes
C25 . C24 . C26 . 109.22(13) yes
C16 . C24 . H241 . 108.1 no
C25 . C24 . H241 . 107.0 no
C26 . C24 . H241 . 109.9 no
C24 . C25 . H251 . 106.0 no
C24 . C25 . H252 . 109.0 no
H251 . C25 . H252 . 110.7 no
C24 . C25 . H253 . 107.7 no
H251 . C25 . H253 . 111.0 no
H252 . C25 . H253 . 112.1 no
C24 . C26 . H261 . 106.8 no
C24 . C26 . H262 . 109.0 no
H261 . C26 . H262 . 111.2 no
C24 . C26 . H263 . 108.7 no
H261 . C26 . H263 . 108.9 no
H262 . C26 . H263 . 112.0 no
N14 . B27 . N28 . 114.57(12) yes
N14 . B27 . C45 . 123.66(12) yes
N28 . B27 . C45 . 121.77(12) yes
B27 . N28 . C29 . 121.55(12) yes
B27 . N28 . C32 . 120.73(12) yes
C29 . N28 . C32 . 117.69(12) yes
N28 . C29 . C30 . 119.23(12) yes
N28 . C29 . C31 . 120.89(13) yes
C30 . C29 . C31 . 119.87(13) yes
C13 . C30 . C29 . 122.98(13) yes
C13 . C30 . H301 . 118.8 no
C29 . C30 . H301 . 118.0 no
C29 . C31 . H311 . 106.0 no
C29 . C31 . H313 . 112.5 no
H311 . C31 . H313 . 110.4 no
C29 . C31 . H312 . 108.1 no
H311 . C31 . H312 . 108.7 no
H313 . C31 . H312 . 110.9 no
N28 . C32 . C33 . 118.68(13) yes
N28 . C32 . C41 . 117.98(13) yes
C33 . C32 . C41 . 123.31(14) yes
C32 . C33 . C34 . 122.64(14) yes
C32 . C33 . C37 . 116.96(16) yes
C34 . C33 . C37 . 120.39(15) yes
C33 . C34 . C35 . 112.31(15) yes
C33 . C34 . C36 . 110.40(17) yes
C35 . C34 . C36 . 110.93(15) yes
C33 . C34 . H341 . 107.4 no
C35 . C34 . H341 . 106.9 no
C36 . C34 . H341 . 108.7 no
C34 . C35 . H352 . 110.0 no
C34 . C35 . H351 . 108.8 no
H352 . C35 . H351 . 109.3 no
C34 . C35 . H353 . 110.9 no
H352 . C35 . H353 . 108.9 no
H351 . C35 . H353 . 108.9 no
C34 . C36 . H361 . 106.1 no
C34 . C36 . H362 . 110.0 no
H361 . C36 . H362 . 111.7 no
C34 . C36 . H363 . 109.1 no
H361 . C36 . H363 . 110.5 no
H362 . C36 . H363 . 109.4 no
C33 . C37 . C38 . 121.03(18) yes
C33 . C37 . H371 . 119.1 no
C38 . C37 . H371 . 119.8 no
C37 . C38 . C40 . 120.13(18) yes
C37 . C38 . H381 . 119.9 no
C40 . C38 . H381 . 120.0 no
C38 . C40 . C41 . 121.42(18) yes
C38 . C40 . H401 . 118.9 no
C41 . C40 . H401 . 119.6 no
C32 . C41 . C40 . 117.12(16) yes
C32 . C41 . C43 . 123.14(15) yes
C40 . C41 . C43 . 119.74(16) yes
C41 . C43 . C42 . 112.44(15) yes
C41 . C43 . C44 . 112.65(18) yes
C42 . C43 . C44 . 109.31(16) yes
C41 . C43 . H431 . 107.6 no
C42 . C43 . H431 . 105.2 no
C44 . C43 . H431 . 109.3 no
C43 . C42 . H421 . 107.2 no
C43 . C42 . H423 . 108.4 no
H421 . C42 . H423 . 110.9 no
C43 . C42 . H422 . 107.6 no
H421 . C42 . H422 . 111.0 no
H423 . C42 . H422 . 111.6 no
C43 . C44 . H441 . 109.6 no
C43 . C44 . H443 . 103.3 no
H441 . C44 . H443 . 108.7 no
C43 . C44 . H442 . 112.9 no
H441 . C44 . H442 . 112.0 no
H443 . C44 . H442 . 109.9 no
B27 . C45 . C46 . 122.77(12) yes
B27 . C45 . C52 . 120.47(13) yes
C46 . C45 . C52 . 116.76(13) yes
C45 . C46 . C47 . 121.70(14) yes
C45 . C46 . H461 . 118.1 no
C47 . C46 . H461 . 120.1 no
C46 . C47 . C48 . 120.29(15) yes
C46 . C47 . H471 . 119.6 no
C48 . C47 . H471 . 120.0 no
C47 . C48 . C49 . 119.46(14) yes
C47 . C48 . H481 . 119.3 no
C49 . C48 . H481 . 121.2 no
C48 . C49 . C52 . 119.98(15) yes
C48 . C49 . H491 . 122.0 no
C52 . C49 . H491 . 118.0 no
C45 . C52 . C49 . 121.78(14) yes
C45 . C52 . H521 . 120.3 no
C49 . C52 . H521 . 117.9 no
B11 . C50 . C51 . 126.81(12) yes
B11 . C50 . C58 . 119.55(12) yes
C51 . C50 . C58 . 113.14(13) yes
C50 . C51 . F52 . 121.14(13) yes
C50 . C51 . C53 . 124.44(14) yes
F52 . C51 . C53 . 114.40(13) yes
C51 . C53 . F54 . 120.87(15) yes
C51 . C53 . C55 . 119.57(15) yes
F54 . C53 . C55 . 119.56(14) yes
C53 . C55 . F56 . 120.28(17) yes
C53 . C55 . C57 . 118.72(15) yes
F56 . C55 . C57 . 121.00(17) yes
C55 . C57 . C58 . 119.54(16) yes
C55 . C57 . F60 . 119.64(16) yes
C58 . C57 . F60 . 120.81(16) yes
C50 . C58 . C57 . 124.54(15) yes
C50 . C58 . F59 . 119.14(13) yes
C57 . C58 . F59 . 116.32(15) yes
B11 . C61 . C62 . 119.00(12) yes
B11 . C61 . C69 . 127.85(13) yes
C62 . C61 . C69 . 112.60(13) yes
C61 . C62 . F63 . 119.11(12) yes
C61 . C62 . C64 . 124.64(15) yes
F63 . C62 . C64 . 116.25(14) yes
C62 . C64 . F65 . 120.69(17) yes
C62 . C64 . C66 . 119.57(16) yes
F65 . C64 . C66 . 119.74(15) yes
C64 . C66 . F67 . 119.93(17) yes
C64 . C66 . C68 . 118.84(15) yes
F67 . C66 . C68 . 121.23(18) yes
C66 . C68 . C69 . 119.75(16) yes
C66 . C68 . F71 . 120.07(15) yes
C69 . C68 . F71 . 120.18(17) yes
C61 . C69 . C68 . 124.51(15) yes
C61 . C69 . F70 . 120.55(13) yes
C68 . C69 . F70 . 114.91(14) yes
C74 . O73 . C76 . 111.60(13) yes
O73 . C74 . C75 . 108.33(16) yes
O73 . C74 . H742 . 113.2 no
C75 . C74 . H742 . 110.8 no
O73 . C74 . H741 . 110.5 no
C75 . C74 . H741 . 108.9 no
H742 . C74 . H741 . 105.0 no
C74 . C75 . H751 . 105.4 no
C74 . C75 . H753 . 107.7 no
H751 . C75 . H753 . 110.7 no
C74 . C75 . H752 . 108.9 no
H751 . C75 . H752 . 110.7 no
H753 . C75 . H752 . 113.2 no
O73 . C76 . C77 . 108.17(17) yes
O73 . C76 . H761 . 108.9 no
C77 . C76 . H761 . 110.3 no
O73 . C76 . H762 . 110.1 no
C77 . C76 . H762 . 109.1 no
H761 . C76 . H762 . 110.2 no
C76 . C77 . H771 . 115.2 no
C76 . C77 . H772 . 106.0 no
H771 . C77 . H772 . 107.5 no
C76 . C77 . H773 . 111.1 no
H771 . C77 . H773 . 109.8 no
H772 . C77 . H773 . 106.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C21 . H211 . C13 . 132.24 0.986 2.452 3.199(2) yes
C31 . H312 . C41 . 130.96 0.970 2.557 3.276(2) yes
C43 . H431 . C29 . 130.36 0.999 2.549 3.286(2) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 26/01/14 at 20:51:48
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 313,X'S) H   ( 312,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 423,X'S) H   ( 422,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 443,X'S) H   ( 442,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) H   ( 753,X'S) H   ( 752,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) H   ( 773,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 26/01/14 at 20:51:48
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.579 -0.030 0.018 192 44 ' '
2 0.079 0.530 0.018 192 44 ' '
3 0.421 0.030 0.518 192 44 ' '
4 0.921 0.470 0.518 192 44 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_104jart13
_database_code_depnum_ccdc_archive 'CCDC 1544787'
_audit_update_record             
;
2017-04-18 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_audit_creation_date             13-09-09
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title '104jart13 in P -1'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   11.3489(3)
_cell_length_b                   12.4418(4)
_cell_length_c                   21.2535(5)
_cell_angle_alpha                77.338(2)
_cell_angle_beta                 81.922(2)
_cell_angle_gamma                81.571(2)
_cell_volume                     2878.07(14)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Al 0.2130 0.2455 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886
1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C46 H54 Al1 B1 F15 N2 O1 
# Dc =      1.12 Fooo =   1170.00 Mu =     10.11 M =    973.71
# Found Formula = C58 H62 Al1 B1 F15 N2 O1 
# Dc =      1.30 FOOO =   1170.00 Mu =     10.87 M =   1125.91

_chemical_formula_sum            'C58 H62 Al1 B1 F15 N2 O1'
_chemical_formula_moiety         'C58 H62 Al1 B1 F15 N2 O1'
_chemical_compound_source        .
_chemical_formula_weight         1125.91


_cell_measurement_reflns_used    12204
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.040
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_max          0.170

_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1170
_exptl_absorpt_coefficient_mu    1.087

# Sheldrick geometric approximatio 0.91 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.96
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            11906
_reflns_number_total             11906
_diffrn_reflns_av_R_equivalents  0.025
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11906 
# Theoretical number of reflections is about 24080 


_diffrn_reflns_theta_min         3.667
_diffrn_reflns_theta_max         76.133
_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        73.849
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              -15
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              26

_oxford_diffrn_Wilson_B_factor   2.80
_oxford_diffrn_Wilson_scale      0.04

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.72
_refine_diff_density_max         0.72


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         11851
_refine_ls_number_restraints     18
_refine_ls_number_parameters     703
_oxford_refine_ls_R_factor_ref   0.0604
_refine_ls_wR_factor_ref         0.1361
_refine_ls_goodness_of_fit_ref   0.9699
_refine_ls_shift/su_max          0.0007158
_refine_ls_shift/su_mean         0.0000470


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11857
_refine_ls_R_factor_all          0.0605
_refine_ls_wR_factor_all         0.1365

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9916
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_gt          0.1285

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 2.36P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Al1 Al 0.66006(5) 0.65016(4) 0.23028(3) 0.0262 1.0000 Uani . . . . . .
O2 O 0.57665(12) 0.67411(12) 0.30981(6) 0.0319 1.0000 Uani . . . . . .
C3 C 0.63062(18) 0.65925(19) 0.37105(10) 0.0369 1.0000 Uani . . . . . .
C4 C 0.5482(2) 0.7343(3) 0.40886(12) 0.0517 1.0000 Uani . . . . . .
C5 C 0.4263(2) 0.7309(2) 0.38908(11) 0.0465 1.0000 Uani . . . . . .
C6 C 0.45148(18) 0.72885(19) 0.31752(10) 0.0378 1.0000 Uani . . . . . .
N7 N 0.80003(14) 0.71637(13) 0.22105(7) 0.0274 1.0000 Uani . . . . . .
C8 C 0.88952(16) 0.66166(15) 0.25590(8) 0.0266 1.0000 Uani . . . . . .
C9 C 0.89408(15) 0.55011(15) 0.28560(8) 0.0251 1.0000 Uani . . . . . .
C10 C 0.82618(15) 0.46912(15) 0.27676(8) 0.0243 1.0000 Uani . . . . . .
N11 N 0.72243(13) 0.49974(12) 0.25017(7) 0.0246 1.0000 Uani . . . . . .
C12 C 0.64990(15) 0.41958(15) 0.23875(9) 0.0264 1.0000 Uani . . . . . .
C13 C 0.64901(17) 0.40555(16) 0.17489(9) 0.0314 1.0000 Uani . . . . . .
C14 C 0.5704(2) 0.33669(18) 0.16427(11) 0.0392 1.0000 Uani . . . . . .
C15 C 0.4937(2) 0.28472(18) 0.21385(12) 0.0413 1.0000 Uani . . . . . .
C16 C 0.49545(18) 0.29899(17) 0.27607(11) 0.0376 1.0000 Uani . . . . . .
C17 C 0.57261(17) 0.36563(16) 0.29004(10) 0.0308 1.0000 Uani . . . . . .
C18 C 0.56696(18) 0.37762(18) 0.35974(10) 0.0355 1.0000 Uani . . . . . .
C19 C 0.5909(2) 0.2648(2) 0.40573(12) 0.0488 1.0000 Uani . . . . . .
C20 C 0.4447(2) 0.4357(2) 0.38253(12) 0.0442 1.0000 Uani . . . . . .
C21 C 0.7295(2) 0.4616(2) 0.11757(10) 0.0401 1.0000 Uani . . . . . .
C22 C 0.6662(3) 0.5010(3) 0.05642(12) 0.0562 1.0000 Uani . . . . . .
C23 C 0.8419(3) 0.3837(4) 0.10432(15) 0.0873 1.0000 Uani . . . . . .
C24 C 0.87367(15) 0.34739(15) 0.29620(8) 0.0256 1.0000 Uani . . . . . .
B25 B 1.00837(17) 0.31116(17) 0.32229(10) 0.0252 1.0000 Uani . . . . . .
C26 C 1.01533(17) 0.33536(15) 0.39554(9) 0.0276 1.0000 Uani . . . . . .
C27 C 1.12264(18) 0.30576(16) 0.42331(9) 0.0321 1.0000 Uani . . . . . .
F28 F 1.22175(10) 0.26634(10) 0.38786(6) 0.0378 1.0000 Uani . . . . . .
C29 C 1.1367(2) 0.31432(18) 0.48515(10) 0.0391 1.0000 Uani . . . . . .
F30 F 1.24440(13) 0.28625(13) 0.50805(7) 0.0542 1.0000 Uani . . . . . .
C31 C 1.0398(2) 0.35210(18) 0.52453(10) 0.0406 1.0000 Uani . . . . . .
F32 F 1.05252(16) 0.36048(13) 0.58494(6) 0.0564 1.0000 Uani . . . . . .
C33 C 0.9310(2) 0.38109(17) 0.50059(10) 0.0366 1.0000 Uani . . . . . .
C34 C 0.92139(18) 0.37272(16) 0.43744(9) 0.0310 1.0000 Uani . . . . . .
F35 F 0.81012(10) 0.40428(11) 0.41887(6) 0.0378 1.0000 Uani . . . . . .
F36 F 0.83466(13) 0.41795(12) 0.53809(6) 0.0497 1.0000 Uani . . . . . .
C37 C 1.10629(15) 0.37257(15) 0.26529(9) 0.0274 1.0000 Uani . . . . . .
C38 C 1.17539(16) 0.45323(16) 0.26979(9) 0.0310 1.0000 Uani . . . . . .
F39 F 1.17028(10) 0.48948(10) 0.32565(6) 0.0346 1.0000 Uani . . . . . .
C40 C 1.25051(18) 0.50503(18) 0.21874(11) 0.0374 1.0000 Uani . . . . . .
F41 F 1.31283(12) 0.58385(12) 0.22744(7) 0.0521 1.0000 Uani . . . . . .
C42 C 1.26078(19) 0.4770(2) 0.15915(11) 0.0418 1.0000 Uani . . . . . .
F43 F 1.33343(13) 0.52687(14) 0.10914(7) 0.0578 1.0000 Uani . . . . . .
C44 C 1.19451(19) 0.39830(19) 0.15152(10) 0.0391 1.0000 Uani . . . . . .
C45 C 1.12060(17) 0.34800(17) 0.20364(9) 0.0321 1.0000 Uani . . . . . .
F46 F 1.06185(11) 0.26813(10) 0.19233(6) 0.0387 1.0000 Uani . . . . . .
F47 F 1.20277(14) 0.36843(14) 0.09364(6) 0.0552 1.0000 Uani . . . . . .
C48 C 1.04204(16) 0.17293(15) 0.33481(9) 0.0290 1.0000 Uani . . . . . .
C49 C 1.14693(18) 0.11397(17) 0.31110(10) 0.0343 1.0000 Uani . . . . . .
F50 F 1.23547(11) 0.16583(10) 0.27309(6) 0.0436 1.0000 Uani . . . . . .
C51 C 1.1724(2) -0.00008(18) 0.32582(12) 0.0434 1.0000 Uani . . . . . .
F52 F 1.27675(14) -0.05024(12) 0.30106(8) 0.0602 1.0000 Uani . . . . . .
C53 C 1.0935(2) -0.06352(18) 0.36737(14) 0.0509 1.0000 Uani . . . . . .
F54 F 1.11876(16) -0.17411(12) 0.38245(10) 0.0718 1.0000 Uani . . . . . .
C55 C 0.9906(2) -0.00985(19) 0.39444(14) 0.0500 1.0000 Uani . . . . . .
C56 C 0.96736(18) 0.10421(17) 0.37772(11) 0.0377 1.0000 Uani . . . . . .
F57 F 0.86527(11) 0.14950(11) 0.40785(7) 0.0484 1.0000 Uani . . . . . .
F58 F 0.91349(15) -0.06994(13) 0.43664(11) 0.0774 1.0000 Uani . . . . . .
C59 C 0.99108(19) 0.72276(17) 0.26203(10) 0.0360 1.0000 Uani . . . . . .
C60 C 0.81916(18) 0.82101(16) 0.17684(10) 0.0328 1.0000 Uani . . . . . .
C61 C 0.8822(2) 0.81826(18) 0.11525(11) 0.0396 1.0000 Uani . . . . . .
C62 C 0.8979(2) 0.9193(2) 0.07262(13) 0.0540 1.0000 Uani . . . . . .
C63 C 0.8541(3) 1.0183(2) 0.08997(15) 0.0638 1.0000 Uani . . . . . .
C64 C 0.7928(3) 1.0202(2) 0.15064(15) 0.0562 1.0000 Uani . . . . . .
C65 C 0.7739(2) 0.92195(18) 0.19518(12) 0.0413 1.0000 Uani . . . . . .
C66 C 0.7047(2) 0.92903(19) 0.26125(13) 0.0486 1.0000 Uani . . . . . .
C67 C 0.7683(4) 0.9899(4) 0.2984(2) 0.0947 1.0000 Uani . . . . . .
C68 C 0.5783(3) 0.9869(2) 0.25380(18) 0.0700 1.0000 Uani . . . . . .
C69 C 0.9333(2) 0.7116(2) 0.09272(10) 0.0456 1.0000 Uani . . . . . .
C70 C 0.8834(3) 0.7044(3) 0.03089(14) 0.0628 1.0000 Uani . . . . . .
C71 C 1.0705(3) 0.6995(3) 0.08105(14) 0.0584 1.0000 Uani . . . . . .
C72 C 0.55304(19) 0.71045(18) 0.16408(10) 0.0373 1.0000 Uani . . . . . .
C76 C 1.4117(4) 0.1216(4) 0.0599(2) 0.1205 1.0000 Uani D . . . . .
C77 C 1.3447(4) 0.0452(4) 0.1042(2) 0.1256 1.0000 Uani D . . . . .
C78 C 1.2262(4) 0.0304(5) 0.1085(3) 0.1612 1.0000 Uani D . . . . .
C79 C 1.1635(5) -0.0459(5) 0.1574(3) 0.1432 1.0000 Uani D . . . . .
C80 C 1.5301(4) 0.1299(4) 0.0521(3) 0.1720 1.0000 Uani D . . . . .
C81 C 1.5946(4) 0.2093(4) 0.0012(2) 0.1015 1.0000 Uani D . . . . .
H31 H 0.7116 0.6793 0.3635 0.0472 1.0000 Uiso R . . . . .
H32 H 0.6345 0.5802 0.3951 0.0471 1.0000 Uiso R . . . . .
H42 H 0.5748 0.8095 0.3944 0.0665 1.0000 Uiso R . . . . .
H41 H 0.5501 0.7060 0.4564 0.0661 1.0000 Uiso R . . . . .
H52 H 0.3680 0.7947 0.3958 0.0601 1.0000 Uiso R . . . . .
H51 H 0.3942 0.6640 0.4125 0.0606 1.0000 Uiso R . . . . .
H61 H 0.4481 0.8070 0.2914 0.0469 1.0000 Uiso R . . . . .
H62 H 0.3937 0.6899 0.3021 0.0475 1.0000 Uiso R . . . . .
H91 H 0.9506 0.5261 0.3154 0.0315 1.0000 Uiso R . . . . .
H141 H 0.5689 0.3244 0.1219 0.0488 1.0000 Uiso R . . . . .
H151 H 0.4409 0.2385 0.2068 0.0483 1.0000 Uiso R . . . . .
H161 H 0.4427 0.2629 0.3092 0.0453 1.0000 Uiso R . . . . .
H181 H 0.6288 0.4230 0.3645 0.0419 1.0000 Uiso R . . . . .
H191 H 0.6087 0.2791 0.4457 0.0752 1.0000 Uiso R . . . . .
H192 H 0.6597 0.2235 0.3853 0.0753 1.0000 Uiso R . . . . .
H193 H 0.5186 0.2293 0.4115 0.0747 1.0000 Uiso R . . . . .
H202 H 0.4492 0.4519 0.4241 0.0671 1.0000 Uiso R . . . . .
H201 H 0.4258 0.5030 0.3523 0.0664 1.0000 Uiso R . . . . .
H203 H 0.3838 0.3858 0.3858 0.0667 1.0000 Uiso R . . . . .
H211 H 0.7532 0.5274 0.1297 0.0502 1.0000 Uiso R . . . . .
H221 H 0.7173 0.5422 0.0205 0.0886 1.0000 Uiso R . . . . .
H222 H 0.5908 0.5469 0.0641 0.0894 1.0000 Uiso R . . . . .
H223 H 0.6491 0.4349 0.0422 0.0894 1.0000 Uiso R . . . . .
H232 H 0.8929 0.4186 0.0678 0.1339 1.0000 Uiso R . . . . .
H231 H 0.8848 0.3618 0.1415 0.1344 1.0000 Uiso R . . . . .
H233 H 0.8211 0.3150 0.0924 0.1344 1.0000 Uiso R . . . . .
H242 H 0.8153 0.3157 0.3285 0.0307 1.0000 Uiso R . . . . .
H241 H 0.8756 0.3157 0.2582 0.0300 1.0000 Uiso R . . . . .
H591 H 1.0452 0.6750 0.2901 0.0581 1.0000 Uiso R . . . . .
H592 H 0.9583 0.7882 0.2801 0.0584 1.0000 Uiso R . . . . .
H593 H 1.0381 0.7421 0.2179 0.0583 1.0000 Uiso R . . . . .
H621 H 0.9388 0.9202 0.0311 0.0652 1.0000 Uiso R . . . . .
H631 H 0.8676 1.0860 0.0595 0.0730 1.0000 Uiso R . . . . .
H641 H 0.7620 1.0885 0.1629 0.0703 1.0000 Uiso R . . . . .
H661 H 0.6993 0.8516 0.2876 0.0597 1.0000 Uiso R . . . . .
H671 H 0.7192 0.9980 0.3385 0.1478 1.0000 Uiso R . . . . .
H672 H 0.7825 1.0635 0.2738 0.1484 1.0000 Uiso R . . . . .
H673 H 0.8446 0.9481 0.3103 0.1480 1.0000 Uiso R . . . . .
H682 H 0.5352 0.9968 0.2964 0.1075 1.0000 Uiso R . . . . .
H681 H 0.5759 1.0605 0.2281 0.1083 1.0000 Uiso R . . . . .
H683 H 0.5284 0.9450 0.2377 0.1083 1.0000 Uiso R . . . . .
H691 H 0.9101 0.6471 0.1289 0.0545 1.0000 Uiso R . . . . .
H701 H 0.9055 0.6294 0.0206 0.0929 1.0000 Uiso R . . . . .
H702 H 0.9188 0.7549 -0.0070 0.0928 1.0000 Uiso R . . . . .
H703 H 0.8001 0.7196 0.0337 0.0933 1.0000 Uiso R . . . . .
H712 H 1.1012 0.6287 0.0661 0.0902 1.0000 Uiso R . . . . .
H711 H 1.1059 0.6969 0.1222 0.0900 1.0000 Uiso R . . . . .
H713 H 1.0983 0.7586 0.0475 0.0903 1.0000 Uiso R . . . . .
H772 H 1.3435 0.0691 0.1444 0.1541 1.0000 Uiso R . . . . .
H771 H 1.3854 -0.0260 0.1027 0.1545 1.0000 Uiso R . . . . .
H781 H 1.1760 0.1074 0.1141 0.1803 1.0000 Uiso R . . . . .
H782 H 1.2119 0.0189 0.0657 0.1805 1.0000 Uiso R . . . . .
H792 H 1.1009 -0.0752 0.1421 0.2121 1.0000 Uiso R . . . . .
H791 H 1.1375 -0.0188 0.1967 0.2122 1.0000 Uiso R . . . . .
H793 H 1.2297 -0.1150 0.1687 0.2125 1.0000 Uiso R . . . . .
H812 H 1.6699 0.2169 0.0165 0.1532 1.0000 Uiso R . . . . .
H811 H 1.5421 0.2768 -0.0054 0.1535 1.0000 Uiso R . . . . .
H813 H 1.6183 0.1826 -0.0414 0.1534 1.0000 Uiso R . . . . .
H761 H 1.3887 0.1925 0.0692 0.1523 1.0000 Uiso R . . . . .
H762 H 1.3921 0.1217 0.0172 0.1523 1.0000 Uiso R . . . . .
H801 H 1.5670 0.1162 0.0887 0.2338 1.0000 Uiso R . . . . .
H802 H 1.5700 0.0494 0.0347 0.2338 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.78(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 . O2 . 1.8790(14) yes
Al1 . N7 . 1.8616(16) yes
Al1 . N11 . 1.8792(16) yes
Al1 . C72 . 1.941(2) yes
O2 . C3 . 1.479(2) yes
O2 . C6 . 1.486(2) yes
C3 . C4 . 1.502(3) yes
C3 . H31 . 0.970 no
C3 . H32 . 1.002 no
C4 . C5 . 1.510(3) yes
C4 . H42 . 0.995 no
C4 . H41 . 0.996 no
C5 . C6 . 1.513(3) yes
C5 . H52 . 0.979 no
C5 . H51 . 0.965 no
C6 . H61 . 1.007 no
C6 . H62 . 0.998 no
N7 . C8 . 1.353(2) yes
N7 . C60 . 1.454(2) yes
C8 . C9 . 1.390(3) yes
C8 . C59 . 1.505(3) yes
C9 . C10 . 1.413(3) yes
C9 . H91 . 0.936 no
C10 . N11 . 1.346(2) yes
C10 . C24 . 1.518(2) yes
N11 . C12 . 1.461(2) yes
C12 . C13 . 1.407(3) yes
C12 . C17 . 1.411(3) yes
C13 . C14 . 1.395(3) yes
C13 . C21 . 1.518(3) yes
C14 . C15 . 1.376(3) yes
C14 . H141 . 0.949 no
C15 . C16 . 1.375(3) yes
C15 . H151 . 0.936 no
C16 . C17 . 1.392(3) yes
C16 . H161 . 0.937 no
C17 . C18 . 1.513(3) yes
C18 . C19 . 1.536(3) yes
C18 . C20 . 1.534(3) yes
C18 . H181 . 0.992 no
C19 . H191 . 0.958 no
C19 . H192 . 0.973 no
C19 . H193 . 0.969 no
C20 . H202 . 0.957 no
C20 . H201 . 0.954 no
C20 . H203 . 0.981 no
C21 . C22 . 1.525(3) yes
C21 . C23 . 1.517(4) yes
C21 . H211 . 0.994 no
C22 . H221 . 0.987 no
C22 . H222 . 0.971 no
C22 . H223 . 0.987 no
C23 . H232 . 0.963 no
C23 . H231 . 0.954 no
C23 . H233 . 1.010 no
C24 . B25 . 1.666(3) yes
C24 . H242 . 0.945 no
C24 . H241 . 0.968 no
B25 . C26 . 1.664(3) yes
B25 . C37 . 1.659(3) yes
B25 . C48 . 1.676(3) yes
C26 . C27 . 1.394(3) yes
C26 . C34 . 1.384(3) yes
C27 . F28 . 1.355(2) yes
C27 . C29 . 1.375(3) yes
C29 . F30 . 1.349(2) yes
C29 . C31 . 1.376(3) yes
C31 . F32 . 1.340(2) yes
C31 . C33 . 1.371(3) yes
C33 . C34 . 1.389(3) yes
C33 . F36 . 1.345(3) yes
C34 . F35 . 1.353(2) yes
C37 . C38 . 1.387(3) yes
C37 . C45 . 1.392(3) yes
C38 . F39 . 1.351(2) yes
C38 . C40 . 1.383(3) yes
C40 . F41 . 1.348(3) yes
C40 . C42 . 1.371(3) yes
C42 . F43 . 1.345(2) yes
C42 . C44 . 1.368(4) yes
C44 . C45 . 1.383(3) yes
C44 . F47 . 1.348(3) yes
C45 . F46 . 1.354(2) yes
C48 . C49 . 1.395(3) yes
C48 . C56 . 1.391(3) yes
C49 . F50 . 1.346(2) yes
C49 . C51 . 1.380(3) yes
C51 . F52 . 1.349(3) yes
C51 . C53 . 1.373(4) yes
C53 . F54 . 1.340(3) yes
C53 . C55 . 1.376(4) yes
C55 . C56 . 1.380(3) yes
C55 . F58 . 1.344(3) yes
C56 . F57 . 1.352(2) yes
C59 . H591 . 0.963 no
C59 . H592 . 0.979 no
C59 . H593 . 1.010 no
C60 . C61 . 1.405(3) yes
C60 . C65 . 1.401(3) yes
C61 . C62 . 1.398(3) yes
C61 . C69 . 1.517(3) yes
C62 . C63 . 1.367(4) yes
C62 . H621 . 0.936 no
C63 . C64 . 1.379(4) yes
C63 . H631 . 0.961 no
C64 . C65 . 1.396(3) yes
C64 . H641 . 0.947 no
C65 . C66 . 1.523(3) yes
C66 . C67 . 1.517(4) yes
C66 . C68 . 1.521(4) yes
C66 . H661 . 1.008 no
C67 . H671 . 0.965 no
C67 . H672 . 0.973 no
C67 . H673 . 0.977 no
C68 . H682 . 0.990 no
C68 . H681 . 0.957 no
C68 . H683 . 0.964 no
C69 . C70 . 1.527(4) yes
C69 . C71 . 1.532(4) yes
C69 . H691 . 1.020 no
C70 . H701 . 0.993 no
C70 . H702 . 0.983 no
C70 . H703 . 0.933 no
C71 . H712 . 0.999 no
C71 . H711 . 1.005 no
C71 . H713 . 0.961 no
C76 . C77 . 1.409(5) yes
C76 . C80 . 1.346(5) yes
C76 . H761 . 0.938 no
C76 . H762 . 0.965 no
C77 . C78 . 1.372(5) yes
C77 . H772 . 0.961 no
C77 . H771 . 0.942 no
C78 . C79 . 1.431(5) yes
C78 . H781 . 1.061 no
C78 . H782 . 0.990 no
C79 . H792 . 0.968 no
C79 . H791 . 0.960 no
C79 . H793 . 1.065 no
C80 . C81 . 1.484(5) yes
C80 . H801 . 0.906 no
C80 . H802 . 1.152 no
C81 . H812 . 0.981 no
C81 . H811 . 0.952 no
C81 . H813 . 1.021 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 . Al1 . N7 . 105.57(7) yes
O2 . Al1 . N11 . 102.70(7) yes
N7 . Al1 . N11 . 100.19(7) yes
O2 . Al1 . C72 . 107.18(8) yes
N7 . Al1 . C72 . 115.83(8) yes
N11 . Al1 . C72 . 123.49(9) yes
Al1 . O2 . C3 . 125.30(11) yes
Al1 . O2 . C6 . 124.26(12) yes
C3 . O2 . C6 . 109.70(14) yes
O2 . C3 . C4 . 104.10(16) yes
O2 . C3 . H31 . 112.0 no
C4 . C3 . H31 . 111.2 no
O2 . C3 . H32 . 111.2 no
C4 . C3 . H32 . 111.0 no
H31 . C3 . H32 . 107.4 no
C3 . C4 . C5 . 103.7(2) yes
C3 . C4 . H42 . 106.8 no
C5 . C4 . H42 . 111.9 no
C3 . C4 . H41 . 110.6 no
C5 . C4 . H41 . 111.2 no
H42 . C4 . H41 . 112.2 no
C4 . C5 . C6 . 103.77(18) yes
C4 . C5 . H52 . 114.0 no
C6 . C5 . H52 . 110.1 no
C4 . C5 . H51 . 110.0 no
C6 . C5 . H51 . 110.1 no
H52 . C5 . H51 . 108.8 no
C5 . C6 . O2 . 104.34(16) yes
C5 . C6 . H61 . 109.8 no
O2 . C6 . H61 . 108.8 no
C5 . C6 . H62 . 113.3 no
O2 . C6 . H62 . 112.5 no
H61 . C6 . H62 . 108.1 no
Al1 . N7 . C8 . 117.72(12) yes
Al1 . N7 . C60 . 123.39(12) yes
C8 . N7 . C60 . 118.85(15) yes
N7 . C8 . C9 . 123.18(17) yes
N7 . C8 . C59 . 119.09(16) yes
C9 . C8 . C59 . 117.72(16) yes
C8 . C9 . C10 . 129.05(16) yes
C8 . C9 . H91 . 114.7 no
C10 . C9 . H91 . 116.3 no
C9 . C10 . N11 . 120.39(16) yes
C9 . C10 . C24 . 118.92(15) yes
N11 . C10 . C24 . 120.68(16) yes
C10 . N11 . Al1 . 120.44(12) yes
C10 . N11 . C12 . 122.67(15) yes
Al1 . N11 . C12 . 116.80(11) yes
N11 . C12 . C13 . 119.03(16) yes
N11 . C12 . C17 . 120.21(16) yes
C13 . C12 . C17 . 120.45(17) yes
C12 . C13 . C14 . 118.03(18) yes
C12 . C13 . C21 . 123.03(18) yes
C14 . C13 . C21 . 118.93(18) yes
C13 . C14 . C15 . 121.9(2) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 118.1 no
C14 . C15 . C16 . 119.5(2) yes
C14 . C15 . H151 . 122.1 no
C16 . C15 . H151 . 118.4 no
C15 . C16 . C17 . 121.41(19) yes
C15 . C16 . H161 . 118.3 no
C17 . C16 . H161 . 120.3 no
C12 . C17 . C16 . 118.65(19) yes
C12 . C17 . C18 . 123.67(17) yes
C16 . C17 . C18 . 117.66(18) yes
C17 . C18 . C19 . 111.83(19) yes
C17 . C18 . C20 . 111.07(17) yes
C19 . C18 . C20 . 109.08(17) yes
C17 . C18 . H181 . 110.8 no
C19 . C18 . H181 . 106.6 no
C20 . C18 . H181 . 107.3 no
C18 . C19 . H191 . 107.3 no
C18 . C19 . H192 . 107.2 no
H191 . C19 . H192 . 110.7 no
C18 . C19 . H193 . 106.7 no
H191 . C19 . H193 . 111.9 no
H192 . C19 . H193 . 112.7 no
C18 . C20 . H202 . 108.2 no
C18 . C20 . H201 . 109.8 no
H202 . C20 . H201 . 109.7 no
C18 . C20 . H203 . 108.7 no
H202 . C20 . H203 . 110.4 no
H201 . C20 . H203 . 110.1 no
C13 . C21 . C22 . 112.55(19) yes
C13 . C21 . C23 . 110.2(2) yes
C22 . C21 . C23 . 110.0(2) yes
C13 . C21 . H211 . 107.2 no
C22 . C21 . H211 . 108.3 no
C23 . C21 . H211 . 108.5 no
C21 . C22 . H221 . 111.7 no
C21 . C22 . H222 . 112.0 no
H221 . C22 . H222 . 109.2 no
C21 . C22 . H223 . 108.1 no
H221 . C22 . H223 . 107.3 no
H222 . C22 . H223 . 108.3 no
C21 . C23 . H232 . 110.5 no
C21 . C23 . H231 . 110.8 no
H232 . C23 . H231 . 109.7 no
C21 . C23 . H233 . 110.7 no
H232 . C23 . H233 . 106.3 no
H231 . C23 . H233 . 108.7 no
C10 . C24 . B25 . 120.06(15) yes
C10 . C24 . H242 . 105.7 no
B25 . C24 . H242 . 109.2 no
C10 . C24 . H241 . 106.3 no
B25 . C24 . H241 . 106.8 no
H242 . C24 . H241 . 108.3 no
C24 . B25 . C26 . 114.16(14) yes
C24 . B25 . C37 . 107.26(14) yes
C26 . B25 . C37 . 113.49(15) yes
C24 . B25 . C48 . 109.85(14) yes
C26 . B25 . C48 . 101.57(14) yes
C37 . B25 . C48 . 110.45(14) yes
B25 . C26 . C27 . 119.45(16) yes
B25 . C26 . C34 . 127.28(16) yes
C27 . C26 . C34 . 112.92(17) yes
C26 . C27 . F28 . 119.13(17) yes
C26 . C27 . C29 . 124.59(19) yes
F28 . C27 . C29 . 116.28(18) yes
C27 . C29 . F30 . 121.0(2) yes
C27 . C29 . C31 . 119.8(2) yes
F30 . C29 . C31 . 119.20(19) yes
C29 . C31 . F32 . 120.2(2) yes
C29 . C31 . C33 . 118.68(19) yes
F32 . C31 . C33 . 121.1(2) yes
C31 . C33 . C34 . 119.6(2) yes
C31 . C33 . F36 . 119.96(19) yes
C34 . C33 . F36 . 120.5(2) yes
C33 . C34 . C26 . 124.46(19) yes
C33 . C34 . F35 . 114.43(17) yes
C26 . C34 . F35 . 121.11(17) yes
B25 . C37 . C38 . 127.62(17) yes
B25 . C37 . C45 . 119.36(17) yes
C38 . C37 . C45 . 112.93(17) yes
C37 . C38 . F39 . 120.98(16) yes
C37 . C38 . C40 . 124.17(19) yes
F39 . C38 . C40 . 114.82(18) yes
C38 . C40 . F41 . 120.0(2) yes
C38 . C40 . C42 . 120.1(2) yes
F41 . C40 . C42 . 119.95(18) yes
C40 . C42 . F43 . 120.6(2) yes
C40 . C42 . C44 . 118.55(18) yes
F43 . C42 . C44 . 120.8(2) yes
C42 . C44 . C45 . 119.8(2) yes
C42 . C44 . F47 . 120.12(19) yes
C45 . C44 . F47 . 120.1(2) yes
C37 . C45 . C44 . 124.4(2) yes
C37 . C45 . F46 . 119.75(17) yes
C44 . C45 . F46 . 115.79(18) yes
B25 . C48 . C49 . 126.95(16) yes
B25 . C48 . C56 . 120.37(17) yes
C49 . C48 . C56 . 112.38(18) yes
C48 . C49 . F50 . 121.70(17) yes
C48 . C49 . C51 . 124.4(2) yes
F50 . C49 . C51 . 113.88(18) yes
C49 . C51 . F52 . 120.4(2) yes
C49 . C51 . C53 . 120.4(2) yes
F52 . C51 . C53 . 119.2(2) yes
C51 . C53 . F54 . 120.5(2) yes
C51 . C53 . C55 . 118.0(2) yes
F54 . C53 . C55 . 121.4(2) yes
C53 . C55 . C56 . 119.9(2) yes
C53 . C55 . F58 . 119.1(2) yes
C56 . C55 . F58 . 121.0(2) yes
C48 . C56 . C55 . 124.9(2) yes
C48 . C56 . F57 . 119.54(18) yes
C55 . C56 . F57 . 115.53(19) yes
C8 . C59 . H591 . 109.9 no
C8 . C59 . H592 . 109.0 no
H591 . C59 . H592 . 109.8 no
C8 . C59 . H593 . 108.6 no
H591 . C59 . H593 . 106.9 no
H592 . C59 . H593 . 112.7 no
N7 . C60 . C61 . 118.51(18) yes
N7 . C60 . C65 . 120.42(18) yes
C61 . C60 . C65 . 121.07(19) yes
C60 . C61 . C62 . 118.0(2) yes
C60 . C61 . C69 . 123.43(18) yes
C62 . C61 . C69 . 118.5(2) yes
C61 . C62 . C63 . 121.4(2) yes
C61 . C62 . H621 . 120.0 no
C63 . C62 . H621 . 118.6 no
C62 . C63 . C64 . 120.1(2) yes
C62 . C63 . H631 . 118.9 no
C64 . C63 . H631 . 121.0 no
C63 . C64 . C65 . 121.0(2) yes
C63 . C64 . H641 . 120.6 no
C65 . C64 . H641 . 118.4 no
C60 . C65 . C64 . 118.3(2) yes
C60 . C65 . C66 . 122.93(19) yes
C64 . C65 . C66 . 118.7(2) yes
C65 . C66 . C67 . 111.2(3) yes
C65 . C66 . C68 . 110.7(2) yes
C67 . C66 . C68 . 109.6(3) yes
C65 . C66 . H661 . 109.0 no
C67 . C66 . H661 . 107.7 no
C68 . C66 . H661 . 108.6 no
C66 . C67 . H671 . 109.1 no
C66 . C67 . H672 . 111.8 no
H671 . C67 . H672 . 108.3 no
C66 . C67 . H673 . 111.6 no
H671 . C67 . H673 . 106.8 no
H672 . C67 . H673 . 109.2 no
C66 . C68 . H682 . 110.9 no
C66 . C68 . H681 . 113.6 no
H682 . C68 . H681 . 104.3 no
C66 . C68 . H683 . 113.6 no
H682 . C68 . H683 . 104.0 no
H681 . C68 . H683 . 109.6 no
C61 . C69 . C70 . 111.4(2) yes
C61 . C69 . C71 . 112.0(2) yes
C70 . C69 . C71 . 109.2(2) yes
C61 . C69 . H691 . 107.6 no
C70 . C69 . H691 . 109.3 no
C71 . C69 . H691 . 107.2 no
C69 . C70 . H701 . 111.2 no
C69 . C70 . H702 . 111.2 no
H701 . C70 . H702 . 104.7 no
C69 . C70 . H703 . 112.7 no
H701 . C70 . H703 . 107.6 no
H702 . C70 . H703 . 109.1 no
C69 . C71 . H712 . 109.9 no
C69 . C71 . H711 . 110.8 no
H712 . C71 . H711 . 107.6 no
C69 . C71 . H713 . 111.3 no
H712 . C71 . H713 . 106.8 no
H711 . C71 . H713 . 110.2 no
C77 . C76 . C80 . 130.15(7) yes
C77 . C76 . H761 . 109.0 no
C80 . C76 . H761 . 94.9 no
C77 . C76 . H762 . 107.0 no
C80 . C76 . H762 . 105.0 no
H761 . C76 . H762 . 109.2 no
C76 . C77 . C78 . 130.15(7) yes
C76 . C77 . H772 . 102.4 no
C78 . C77 . H772 . 99.0 no
C76 . C77 . H771 . 106.8 no
C78 . C77 . H771 . 103.5 no
H772 . C77 . H771 . 115.4 no
C77 . C78 . C79 . 126.47(7) yes
C77 . C78 . H781 . 106.4 no
C79 . C78 . H781 . 101.5 no
C77 . C78 . H782 . 107.1 no
C79 . C78 . H782 . 107.8 no
H781 . C78 . H782 . 105.9 no
C78 . C79 . H792 . 114.0 no
C78 . C79 . H791 . 113.2 no
H792 . C79 . H791 . 113.2 no
C78 . C79 . H793 . 103.5 no
H792 . C79 . H793 . 104.8 no
H791 . C79 . H793 . 107.0 no
C76 . C80 . C81 . 126.53(7) yes
C76 . C80 . H801 . 116.7 no
C81 . C80 . H801 . 108.9 no
C76 . C80 . H802 . 102.1 no
C81 . C80 . H802 . 98.4 no
H801 . C80 . H802 . 97.1 no
C80 . C81 . H812 . 108.2 no
C80 . C81 . H811 . 106.3 no
H812 . C81 . H811 . 113.1 no
C80 . C81 . H813 . 113.3 no
H812 . C81 . H813 . 105.9 no
H811 . C81 . H813 . 110.3 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 09/09/13 at 20:01:19
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) H   ( 593,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 672,X'S) H   ( 673,X'S) 
RIDE C   (  68,X'S) H   ( 682,X'S) H   ( 681,X'S) H   ( 683,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) H   ( 703,X'S) 
RIDE C   (  71,X'S) H   ( 712,X'S) H   ( 711,X'S) H   ( 713,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  77,X'S) H   ( 772,X'S) H   ( 771,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 792,X'S) H   ( 791,X'S) H   ( 793,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) H   ( 802,X'S) 
RIDE C   (  81,X'S) H   ( 812,X'S) H   ( 811,X'S) H   ( 813,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 09/09/13 at 20:01:19
#
#LIST     16                                                                    
SAME  C(79)  C(78)  C(77)  C(76)  C(80)  C(81) AND 
CONT  C(81)  C(80)  C(76)  C(77)  C(78)  C(79) 
END                                                                             
;


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.500 143 38 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_149JART14
_database_code_depnum_ccdc_archive 'CCDC 1544790'
_audit_update_record             
;
2017-04-18 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_audit_creation_date             2014-01-26
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '149JART14 in C 2/c'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   20.4925(2)
_cell_length_b                   10.74260(10)
_cell_length_c                   37.1031(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.3411(5)
_cell_angle_gamma                90
_cell_volume                     8154.09(16)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C40 H1.25 B2 Cl3 F5 N2 
# Dc =      1.19 Fooo =   3616.00 Mu =      2.75 M =    732.68
# Found Formula = C41 H41 B2 Cl3 F10 N2 
# Dc =      1.43 FOOO =   3616.00 Mu =      3.04 M =    879.75

_chemical_formula_sum            'C41 H41 B2 Cl3 F10 N2'
_chemical_formula_moiety         'C41 H41 B2 Cl3 F10 N2'
_chemical_compound_source        .
_chemical_formula_weight         879.75


_cell_measurement_reflns_used    9012
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_max          0.260

_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3616
_exptl_absorpt_coefficient_mu    0.304

# Sheldrick geometric approximatio 0.94 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.96
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            70816
_reflns_number_total             9182
_diffrn_reflns_av_R_equivalents  0.046
# Number of reflections without Friedels Law is 16707 
# Number of reflections with Friedels Law is 9182 
# Theoretical number of reflections is about 9355 


_diffrn_reflns_theta_min         5.103
_diffrn_reflns_theta_max         27.488
_diffrn_measured_fraction_theta_max 0.983

_diffrn_reflns_theta_full        25.014
_diffrn_measured_fraction_theta_full 0.984


_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_reflns_limit_h_min              -26
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              48

_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      96.02

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.80
_refine_diff_density_max         0.68


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         9182
_refine_ls_number_restraints     0
_refine_ls_number_parameters     523
_oxford_refine_ls_R_factor_ref   0.0985
_refine_ls_wR_factor_ref         0.1031
_refine_ls_goodness_of_fit_ref   0.9876
_refine_ls_shift/su_max          0.0012576
_refine_ls_shift/su_mean         0.0000541


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9182
_refine_ls_R_factor_all          0.0985
_refine_ls_wR_factor_all         0.1031

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5818
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_gt          0.0764

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 4.64 4.92 1.24 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cl1 Cl 0.56954(4) 0.72871(9) 0.59850(2) 0.0381 1.0000 Uani . . . . . .
B2 B 0.48179(19) 0.7385(4) 0.58108(10) 0.0314 1.0000 Uani . . . . . .
Cl3 Cl 0.42790(5) 0.68518(9) 0.61748(3) 0.0420 1.0000 Uani . . . . . .
Cl4 Cl 0.46971(5) 0.62687(9) 0.54325(3) 0.0486 1.0000 Uani . . . . . .
C5 C 0.46487(15) 0.8828(3) 0.57144(8) 0.0265 1.0000 Uani . . . . . .
C6 C 0.46569(16) 0.9709(3) 0.59873(8) 0.0278 1.0000 Uani . . . . . .
F7 F 0.48353(10) 0.9389(2) 0.63320(5) 0.0395 1.0000 Uani . . . . . .
C8 C 0.44977(16) 1.0947(3) 0.59372(9) 0.0305 1.0000 Uani . . . . . .
F9 F 0.45114(10) 1.17373(19) 0.62203(5) 0.0401 1.0000 Uani . . . . . .
C10 C 0.43190(15) 1.1372(3) 0.55971(9) 0.0290 1.0000 Uani . . . . . .
F11 F 0.41501(10) 1.25737(19) 0.55466(6) 0.0402 1.0000 Uani . . . . . .
C12 C 0.43074(16) 1.0557(3) 0.53143(9) 0.0293 1.0000 Uani . . . . . .
C13 C 0.44777(15) 0.9318(3) 0.53764(8) 0.0273 1.0000 Uani . . . . . .
F14 F 0.44517(10) 0.8606(2) 0.50752(5) 0.0376 1.0000 Uani . . . . . .
F15 F 0.41223(10) 1.0943(2) 0.49801(5) 0.0426 1.0000 Uani . . . . . .
F16 F 0.71351(9) 0.66643(18) 0.63296(5) 0.0311 1.0000 Uani . . . . . .
C17 C 0.75747(14) 0.5872(3) 0.64857(8) 0.0242 1.0000 Uani . . . . . .
C18 C 0.73999(14) 0.4633(3) 0.65246(7) 0.0225 1.0000 Uani . . . . . .
C19 C 0.78780(15) 0.3879(3) 0.66894(8) 0.0277 1.0000 Uani . . . . . .
F20 F 0.77634(9) 0.26594(19) 0.67373(6) 0.0389 1.0000 Uani . . . . . .
C21 C 0.84835(15) 0.4324(3) 0.68170(8) 0.0285 1.0000 Uani . . . . . .
F22 F 0.89181(9) 0.3570(2) 0.69873(5) 0.0405 1.0000 Uani . . . . . .
C23 C 0.86259(15) 0.5568(3) 0.67762(8) 0.0280 1.0000 Uani . . . . . .
C24 C 0.81742(15) 0.6349(3) 0.66040(8) 0.0260 1.0000 Uani . . . . . .
F25 F 0.83101(9) 0.75564(18) 0.65629(5) 0.0362 1.0000 Uani . . . . . .
F26 F 0.91975(9) 0.6016(2) 0.69121(5) 0.0367 1.0000 Uani . . . . . .
B27 B 0.66808(16) 0.4244(3) 0.63886(9) 0.0212 1.0000 Uani . . . . . .
N28 N 0.61451(12) 0.4341(2) 0.66222(6) 0.0206 1.0000 Uani . . . . . .
C29 C 0.55147(14) 0.4225(3) 0.64839(8) 0.0217 1.0000 Uani . . . . . .
C30 C 0.53981(14) 0.4013(3) 0.61175(8) 0.0233 1.0000 Uani . . . . . .
C31 C 0.58931(14) 0.3813(3) 0.58875(8) 0.0222 1.0000 Uani . . . . . .
N32 N 0.65296(11) 0.3886(2) 0.60201(6) 0.0206 1.0000 Uani . . . . . .
C33 C 0.70554(14) 0.3519(3) 0.57862(8) 0.0222 1.0000 Uani . . . . . .
C34 C 0.72946(14) 0.4387(3) 0.55453(8) 0.0237 1.0000 Uani . . . . . .
C35 C 0.77900(15) 0.3987(3) 0.53317(9) 0.0299 1.0000 Uani . . . . . .
C36 C 0.80320(16) 0.2790(3) 0.53572(9) 0.0329 1.0000 Uani . . . . . .
C37 C 0.77818(16) 0.1953(3) 0.55950(9) 0.0309 1.0000 Uani . . . . . .
C38 C 0.72790(15) 0.2283(3) 0.58122(8) 0.0248 1.0000 Uani . . . . . .
C39 C 0.69823(17) 0.1301(3) 0.60502(9) 0.0340 1.0000 Uani . . . . . .
C40 C 0.7480(2) 0.0364(4) 0.62065(11) 0.0494 1.0000 Uani . . . . . .
C41 C 0.6427(2) 0.0618(4) 0.58444(14) 0.0651 1.0000 Uani . . . . . .
C42 C 0.70396(16) 0.5709(3) 0.55013(9) 0.0298 1.0000 Uani . . . . . .
C43 C 0.67087(19) 0.5923(4) 0.51243(10) 0.0451 1.0000 Uani . . . . . .
C44 C 0.75866(18) 0.6671(3) 0.55642(10) 0.0381 1.0000 Uani . . . . . .
C45 C 0.57338(15) 0.3534(3) 0.54997(8) 0.0292 1.0000 Uani . . . . . .
C46 C 0.49515(15) 0.4352(3) 0.67166(8) 0.0280 1.0000 Uani . . . . . .
C47 C 0.62622(14) 0.4486(3) 0.70156(8) 0.0223 1.0000 Uani . . . . . .
C48 C 0.62236(15) 0.5674(3) 0.71713(8) 0.0239 1.0000 Uani . . . . . .
C49 C 0.63140(16) 0.5749(3) 0.75470(8) 0.0299 1.0000 Uani . . . . . .
C50 C 0.64396(17) 0.4701(3) 0.77545(9) 0.0336 1.0000 Uani . . . . . .
C51 C 0.64742(16) 0.3551(3) 0.75920(8) 0.0304 1.0000 Uani . . . . . .
C52 C 0.63859(14) 0.3403(3) 0.72190(8) 0.0240 1.0000 Uani . . . . . .
C53 C 0.64049(16) 0.2106(3) 0.70574(9) 0.0288 1.0000 Uani . . . . . .
C54 C 0.57355(18) 0.1492(4) 0.70385(12) 0.0482 1.0000 Uani . . . . . .
C55 C 0.69053(18) 0.1252(3) 0.72541(10) 0.0380 1.0000 Uani . . . . . .
C56 C 0.60928(16) 0.6859(3) 0.69564(9) 0.0300 1.0000 Uani . . . . . .
C57 C 0.54517(18) 0.7481(4) 0.70505(10) 0.0412 1.0000 Uani . . . . . .
C58 C 0.66512(19) 0.7795(3) 0.70205(10) 0.0410 1.0000 Uani . . . . . .
H301 H 0.4959 0.4002 0.6020 0.0302 1.0000 Uiso R . . . . .
H351 H 0.7965 0.4552 0.5166 0.0370 1.0000 Uiso R . . . . .
H361 H 0.8371 0.2539 0.5209 0.0401 1.0000 Uiso R . . . . .
H371 H 0.7956 0.1135 0.5612 0.0391 1.0000 Uiso R . . . . .
H391 H 0.6803 0.1721 0.6247 0.0437 1.0000 Uiso R . . . . .
H401 H 0.7271 -0.0219 0.6354 0.0624 1.0000 Uiso R . . . . .
H403 H 0.7813 0.0787 0.6347 0.0624 1.0000 Uiso R . . . . .
H402 H 0.7668 -0.0061 0.6014 0.0624 1.0000 Uiso R . . . . .
H412 H 0.6244 0.0017 0.5996 0.0804 1.0000 Uiso R . . . . .
H411 H 0.6594 0.0215 0.5641 0.0804 1.0000 Uiso R . . . . .
H413 H 0.6099 0.1198 0.5765 0.0804 1.0000 Uiso R . . . . .
H421 H 0.6725 0.5843 0.5675 0.0387 1.0000 Uiso R . . . . .
H432 H 0.6551 0.6753 0.5105 0.0561 1.0000 Uiso R . . . . .
H433 H 0.7018 0.5784 0.4947 0.0561 1.0000 Uiso R . . . . .
H431 H 0.6354 0.5359 0.5087 0.0561 1.0000 Uiso R . . . . .
H441 H 0.7412 0.7486 0.5537 0.0485 1.0000 Uiso R . . . . .
H443 H 0.7782 0.6577 0.5801 0.0485 1.0000 Uiso R . . . . .
H442 H 0.7907 0.6542 0.5393 0.0485 1.0000 Uiso R . . . . .
H452 H 0.6124 0.3419 0.5378 0.0379 1.0000 Uiso R . . . . .
H451 H 0.5478 0.2797 0.5480 0.0379 1.0000 Uiso R . . . . .
H453 H 0.5493 0.4210 0.5394 0.0379 1.0000 Uiso R . . . . .
H463 H 0.4554 0.4248 0.6575 0.0360 1.0000 Uiso R . . . . .
H461 H 0.4983 0.3735 0.6900 0.0360 1.0000 Uiso R . . . . .
H462 H 0.4960 0.5155 0.6824 0.0360 1.0000 Uiso R . . . . .
H491 H 0.6288 0.6538 0.7661 0.0383 1.0000 Uiso R . . . . .
H501 H 0.6501 0.4771 0.8009 0.0417 1.0000 Uiso R . . . . .
H511 H 0.6560 0.2836 0.7738 0.0391 1.0000 Uiso R . . . . .
H531 H 0.6531 0.2192 0.6816 0.0366 1.0000 Uiso R . . . . .
H542 H 0.5760 0.0686 0.6934 0.0616 1.0000 Uiso R . . . . .
H541 H 0.5592 0.1422 0.7277 0.0616 1.0000 Uiso R . . . . .
H543 H 0.5435 0.1987 0.6897 0.0616 1.0000 Uiso R . . . . .
H553 H 0.6900 0.0457 0.7142 0.0478 1.0000 Uiso R . . . . .
H551 H 0.6794 0.1165 0.7498 0.0478 1.0000 Uiso R . . . . .
H552 H 0.7330 0.1604 0.7248 0.0478 1.0000 Uiso R . . . . .
H561 H 0.6060 0.6650 0.6707 0.0379 1.0000 Uiso R . . . . .
H571 H 0.5382 0.8216 0.6911 0.0515 1.0000 Uiso R . . . . .
H573 H 0.5477 0.7688 0.7300 0.0515 1.0000 Uiso R . . . . .
H572 H 0.5099 0.6921 0.7001 0.0515 1.0000 Uiso R . . . . .
H582 H 0.6560 0.8526 0.6882 0.0513 1.0000 Uiso R . . . . .
H581 H 0.6692 0.8004 0.7270 0.0513 1.0000 Uiso R . . . . .
H583 H 0.7048 0.7435 0.6951 0.0513 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.094162(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 . B2 . 1.878(4) yes
B2 . Cl3 . 1.883(4) yes
B2 . Cl4 . 1.852(4) yes
B2 . C5 . 1.624(5) yes
C5 . C6 . 1.385(4) yes
C5 . C13 . 1.386(4) yes
C6 . F7 . 1.354(3) yes
C6 . C8 . 1.380(5) yes
C8 . F9 . 1.350(4) yes
C8 . C10 . 1.371(4) yes
C10 . F11 . 1.347(4) yes
C10 . C12 . 1.366(5) yes
C12 . C13 . 1.392(5) yes
C12 . F15 . 1.341(3) yes
C13 . F14 . 1.353(4) yes
F16 . C17 . 1.346(3) yes
C17 . C18 . 1.388(4) yes
C17 . C24 . 1.379(4) yes
C18 . C19 . 1.385(4) yes
C18 . B27 . 1.585(4) yes
C19 . F20 . 1.345(4) yes
C19 . C21 . 1.387(4) yes
C21 . F22 . 1.336(4) yes
C21 . C23 . 1.377(5) yes
C23 . C24 . 1.378(4) yes
C23 . F26 . 1.338(3) yes
C24 . F25 . 1.338(4) yes
B27 . N28 . 1.441(4) yes
B27 . N32 . 1.437(4) yes
N28 . C29 . 1.368(4) yes
N28 . C47 . 1.473(4) yes
C29 . C30 . 1.385(4) yes
C29 . C46 . 1.487(4) yes
C30 . C31 . 1.380(4) yes
C30 . H301 . 0.950 no
C31 . N32 . 1.369(4) yes
C31 . C45 . 1.488(4) yes
N32 . C33 . 1.476(4) yes
C33 . C34 . 1.400(4) yes
C33 . C38 . 1.406(4) yes
C34 . C35 . 1.392(4) yes
C34 . C42 . 1.519(4) yes
C35 . C36 . 1.379(5) yes
C35 . H351 . 0.950 no
C36 . C37 . 1.379(5) yes
C36 . H361 . 0.950 no
C37 . C38 . 1.390(4) yes
C37 . H371 . 0.950 no
C38 . C39 . 1.525(4) yes
C39 . C40 . 1.522(5) yes
C39 . C41 . 1.521(5) yes
C39 . H391 . 0.950 no
C40 . H401 . 0.950 no
C40 . H403 . 0.950 no
C40 . H402 . 0.950 no
C41 . H412 . 0.950 no
C41 . H411 . 0.950 no
C41 . H413 . 0.950 no
C42 . C43 . 1.536(5) yes
C42 . C44 . 1.532(4) yes
C42 . H421 . 0.950 no
C43 . H432 . 0.950 no
C43 . H433 . 0.950 no
C43 . H431 . 0.950 no
C44 . H441 . 0.950 no
C44 . H443 . 0.950 no
C44 . H442 . 0.950 no
C45 . H452 . 0.950 no
C45 . H451 . 0.950 no
C45 . H453 . 0.950 no
C46 . H463 . 0.950 no
C46 . H461 . 0.950 no
C46 . H462 . 0.950 no
C47 . C48 . 1.405(4) yes
C47 . C52 . 1.402(4) yes
C48 . C49 . 1.398(4) yes
C48 . C56 . 1.517(4) yes
C49 . C50 . 1.379(5) yes
C49 . H491 . 0.950 no
C50 . C51 . 1.379(5) yes
C50 . H501 . 0.950 no
C51 . C52 . 1.394(4) yes
C51 . H511 . 0.950 no
C52 . C53 . 1.518(4) yes
C53 . C54 . 1.520(5) yes
C53 . C55 . 1.530(4) yes
C53 . H531 . 0.950 no
C54 . H542 . 0.950 no
C54 . H541 . 0.950 no
C54 . H543 . 0.950 no
C55 . H553 . 0.950 no
C55 . H551 . 0.950 no
C55 . H552 . 0.950 no
C56 . C57 . 1.533(5) yes
C56 . C58 . 1.532(5) yes
C56 . H561 . 0.950 no
C57 . H571 . 0.950 no
C57 . H573 . 0.950 no
C57 . H572 . 0.950 no
C58 . H582 . 0.950 no
C58 . H581 . 0.950 no
C58 . H583 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . B2 . Cl3 . 109.02(19) yes
Cl1 . B2 . Cl4 . 107.9(2) yes
Cl3 . B2 . Cl4 . 106.8(2) yes
Cl1 . B2 . C5 . 108.5(2) yes
Cl3 . B2 . C5 . 108.8(2) yes
Cl4 . B2 . C5 . 115.7(2) yes
B2 . C5 . C6 . 119.8(3) yes
B2 . C5 . C13 . 127.0(3) yes
C6 . C5 . C13 . 113.2(3) yes
C5 . C6 . F7 . 120.5(3) yes
C5 . C6 . C8 . 124.6(3) yes
F7 . C6 . C8 . 114.9(3) yes
C6 . C8 . F9 . 120.5(3) yes
C6 . C8 . C10 . 119.6(3) yes
F9 . C8 . C10 . 119.9(3) yes
C8 . C10 . F11 . 120.0(3) yes
C8 . C10 . C12 . 119.0(3) yes
F11 . C10 . C12 . 121.0(3) yes
C10 . C12 . C13 . 119.5(3) yes
C10 . C12 . F15 . 120.2(3) yes
C13 . C12 . F15 . 120.2(3) yes
C12 . C13 . C5 . 124.1(3) yes
C12 . C13 . F14 . 114.0(3) yes
C5 . C13 . F14 . 121.9(3) yes
F16 . C17 . C18 . 118.8(3) yes
F16 . C17 . C24 . 117.6(3) yes
C18 . C17 . C24 . 123.6(3) yes
C17 . C18 . C19 . 115.2(3) yes
C17 . C18 . B27 . 117.4(3) yes
C19 . C18 . B27 . 127.4(3) yes
C18 . C19 . F20 . 120.2(3) yes
C18 . C19 . C21 . 123.0(3) yes
F20 . C19 . C21 . 116.8(3) yes
C19 . C21 . F22 . 120.7(3) yes
C19 . C21 . C23 . 119.2(3) yes
F22 . C21 . C23 . 120.1(3) yes
C21 . C23 . C24 . 120.0(3) yes
C21 . C23 . F26 . 119.6(3) yes
C24 . C23 . F26 . 120.3(3) yes
C17 . C24 . C23 . 118.9(3) yes
C17 . C24 . F25 . 120.8(3) yes
C23 . C24 . F25 . 120.3(3) yes
C18 . B27 . N28 . 121.1(3) yes
C18 . B27 . N32 . 121.2(3) yes
N28 . B27 . N32 . 117.5(3) yes
B27 . N28 . C29 . 120.2(2) yes
B27 . N28 . C47 . 121.2(2) yes
C29 . N28 . C47 . 118.5(2) yes
N28 . C29 . C30 . 119.2(3) yes
N28 . C29 . C46 . 121.4(3) yes
C30 . C29 . C46 . 119.3(3) yes
C29 . C30 . C31 . 122.8(3) yes
C29 . C30 . H301 . 118.7 no
C31 . C30 . H301 . 118.5 no
C30 . C31 . N32 . 119.2(3) yes
C30 . C31 . C45 . 120.1(3) yes
N32 . C31 . C45 . 120.7(3) yes
C31 . N32 . B27 . 120.3(3) yes
C31 . N32 . C33 . 119.1(2) yes
B27 . N32 . C33 . 120.5(2) yes
N32 . C33 . C34 . 119.5(3) yes
N32 . C33 . C38 . 117.3(3) yes
C34 . C33 . C38 . 123.2(3) yes
C33 . C34 . C35 . 116.9(3) yes
C33 . C34 . C42 . 124.1(3) yes
C35 . C34 . C42 . 119.0(3) yes
C34 . C35 . C36 . 121.3(3) yes
C34 . C35 . H351 . 119.2 no
C36 . C35 . H351 . 119.5 no
C35 . C36 . C37 . 120.4(3) yes
C35 . C36 . H361 . 119.8 no
C37 . C36 . H361 . 119.9 no
C36 . C37 . C38 . 121.4(3) yes
C36 . C37 . H371 . 119.5 no
C38 . C37 . H371 . 119.1 no
C33 . C38 . C37 . 116.8(3) yes
C33 . C38 . C39 . 123.6(3) yes
C37 . C38 . C39 . 119.5(3) yes
C38 . C39 . C40 . 113.4(3) yes
C38 . C39 . C41 . 110.8(3) yes
C40 . C39 . C41 . 109.7(3) yes
C38 . C39 . H391 . 107.5 no
C40 . C39 . H391 . 107.5 no
C41 . C39 . H391 . 107.7 no
C39 . C40 . H401 . 109.9 no
C39 . C40 . H403 . 109.7 no
H401 . C40 . H403 . 109.5 no
C39 . C40 . H402 . 108.8 no
H401 . C40 . H402 . 109.5 no
H403 . C40 . H402 . 109.5 no
C39 . C41 . H412 . 109.9 no
C39 . C41 . H411 . 109.0 no
H412 . C41 . H411 . 109.5 no
C39 . C41 . H413 . 109.6 no
H412 . C41 . H413 . 109.5 no
H411 . C41 . H413 . 109.5 no
C34 . C42 . C43 . 111.6(3) yes
C34 . C42 . C44 . 111.7(3) yes
C43 . C42 . C44 . 108.6(3) yes
C34 . C42 . H421 . 108.1 no
C43 . C42 . H421 . 108.4 no
C44 . C42 . H421 . 108.3 no
C42 . C43 . H432 . 109.8 no
C42 . C43 . H433 . 109.2 no
H432 . C43 . H433 . 109.5 no
C42 . C43 . H431 . 109.4 no
H432 . C43 . H431 . 109.5 no
H433 . C43 . H431 . 109.5 no
C42 . C44 . H441 . 109.7 no
C42 . C44 . H443 . 109.5 no
H441 . C44 . H443 . 109.5 no
C42 . C44 . H442 . 109.2 no
H441 . C44 . H442 . 109.5 no
H443 . C44 . H442 . 109.5 no
C31 . C45 . H452 . 110.1 no
C31 . C45 . H451 . 109.3 no
H452 . C45 . H451 . 109.5 no
C31 . C45 . H453 . 109.0 no
H452 . C45 . H453 . 109.5 no
H451 . C45 . H453 . 109.5 no
C29 . C46 . H463 . 109.8 no
C29 . C46 . H461 . 109.2 no
H463 . C46 . H461 . 109.5 no
C29 . C46 . H462 . 109.4 no
H463 . C46 . H462 . 109.5 no
H461 . C46 . H462 . 109.5 no
N28 . C47 . C48 . 119.6(3) yes
N28 . C47 . C52 . 117.3(3) yes
C48 . C47 . C52 . 123.0(3) yes
C47 . C48 . C49 . 117.0(3) yes
C47 . C48 . C56 . 123.9(3) yes
C49 . C48 . C56 . 119.0(3) yes
C48 . C49 . C50 . 121.3(3) yes
C48 . C49 . H491 . 119.1 no
C50 . C49 . H491 . 119.6 no
C49 . C50 . C51 . 120.0(3) yes
C49 . C50 . H501 . 120.1 no
C51 . C50 . H501 . 119.9 no
C50 . C51 . C52 . 121.9(3) yes
C50 . C51 . H511 . 119.2 no
C52 . C51 . H511 . 118.9 no
C47 . C52 . C51 . 116.7(3) yes
C47 . C52 . C53 . 123.8(3) yes
C51 . C52 . C53 . 119.5(3) yes
C52 . C53 . C54 . 111.9(3) yes
C52 . C53 . C55 . 113.2(3) yes
C54 . C53 . C55 . 109.8(3) yes
C52 . C53 . H531 . 107.3 no
C54 . C53 . H531 . 107.0 no
C55 . C53 . H531 . 107.2 no
C53 . C54 . H542 . 110.2 no
C53 . C54 . H541 . 108.6 no
H542 . C54 . H541 . 109.5 no
C53 . C54 . H543 . 109.6 no
H542 . C54 . H543 . 109.5 no
H541 . C54 . H543 . 109.5 no
C53 . C55 . H553 . 109.8 no
C53 . C55 . H551 . 108.8 no
H553 . C55 . H551 . 109.5 no
C53 . C55 . H552 . 109.8 no
H553 . C55 . H552 . 109.5 no
H551 . C55 . H552 . 109.5 no
C48 . C56 . C57 . 112.0(3) yes
C48 . C56 . C58 . 111.2(3) yes
C57 . C56 . C58 . 108.7(3) yes
C48 . C56 . H561 . 108.3 no
C57 . C56 . H561 . 108.2 no
C58 . C56 . H561 . 108.4 no
C56 . C57 . H571 . 110.0 no
C56 . C57 . H573 . 109.0 no
H571 . C57 . H573 . 109.5 no
C56 . C57 . H572 . 109.4 no
H571 . C57 . H572 . 109.5 no
H573 . C57 . H572 . 109.5 no
C56 . C58 . H582 . 109.7 no
C56 . C58 . H581 . 109.2 no
H582 . C58 . H581 . 109.5 no
C56 . C58 . H583 . 109.5 no
H582 . C58 . H583 . 109.5 no
H581 . C58 . H583 . 109.5 no


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 26/01/14 at 10:53:00
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 403,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 412,X'S) H   ( 411,X'S) H   ( 413,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 433,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 443,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 452,X'S) H   ( 451,X'S) H   ( 453,X'S) 
RIDE C   (  46,X'S) H   ( 463,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) H   ( 543,X'S) 
RIDE C   (  55,X'S) H   ( 553,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 573,X'S) H   ( 572,X'S) 
RIDE C   (  58,X'S) H   ( 582,X'S) H   ( 581,X'S) H   ( 583,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 26/01/14 at 10:53:00
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_120jart13
_database_code_depnum_ccdc_archive 'CCDC 1544791'
_audit_update_record             
;
2017-04-18 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_audit_creation_date             13-10-23
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title '120jart13 in P b c a'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   19.1181(2)
_cell_length_b                   19.0706(2)
_cell_length_c                   21.2422(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7744.77(14)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C45 H56.25 B2.25 Cl2.25 N4.50 
# Dc =      1.31 Fooo =   2976.00 Mu =     19.62 M =    764.32
# Found Formula = C41 H51 B2 Cl3 N2 
# Dc =      1.20 FOOO =   2976.00 Mu =     23.62 M =    699.85

_chemical_formula_sum            'C41 H51 B2 Cl3 N2'
_chemical_formula_moiety         'C41 H51 B2 Cl3 N2'
_chemical_compound_source        .
_chemical_formula_weight         699.85


_cell_measurement_reflns_used    24867
_cell_measurement_theta_min      3
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.050
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_max          0.120

_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2976
_exptl_absorpt_coefficient_mu    2.362

# Sheldrick geometric approximatio 0.79 0.89 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.89
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            86558
_reflns_number_total             8079
_diffrn_reflns_av_R_equivalents  0.071
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8079 
# Theoretical number of reflections is about 16233 


_diffrn_reflns_theta_min         3.879
_diffrn_reflns_theta_max         76.295
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        76.295
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              0
_reflns_limit_h_max              23
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              26

_oxford_diffrn_Wilson_B_factor   2.44
_oxford_diffrn_Wilson_scale      0.22

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.34
_refine_diff_density_max         0.52


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         8048
_refine_ls_number_restraints     68
_refine_ls_number_parameters     452
_oxford_refine_ls_R_factor_ref   0.0502
_refine_ls_wR_factor_ref         0.0994
_refine_ls_goodness_of_fit_ref   1.0381
_refine_ls_shift/su_max          0.0009746
_refine_ls_shift/su_mean         0.0000443


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8048
_refine_ls_R_factor_all          0.0502
_refine_ls_wR_factor_all         0.0994

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6599
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_gt          0.0939

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.03P)² + 5.61P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cl1 Cl -0.00698(2) 0.79728(2) 0.74614(2) 0.0341 1.0000 Uani . . . . . .
B2 B 0.01045(10) 0.70040(11) 0.75299(10) 0.0260 1.0000 Uani . . . . . .
Cl3 Cl -0.05636(3) 0.65493(3) 0.70206(2) 0.0396 1.0000 Uani . . . . . .
Cl4 Cl 0.09970(2) 0.68387(3) 0.71832(2) 0.0365 1.0000 Uani . . . . . .
C5 C 0.00354(9) 0.67372(10) 0.82386(9) 0.0264 1.0000 Uani . . . . . .
C6 C 0.05060(11) 0.62777(11) 0.85230(10) 0.0354 1.0000 Uani . . . . . .
C7 C 0.04000(12) 0.60207(13) 0.91280(10) 0.0429 1.0000 Uani . . . . . .
C8 C -0.01812(12) 0.62211(13) 0.94698(10) 0.0419 1.0000 Uani . . . . . .
C9 C -0.06488(11) 0.66887(14) 0.92040(10) 0.0445 1.0000 Uani . . . . . .
C10 C -0.05391(10) 0.69396(12) 0.85990(10) 0.0361 1.0000 Uani . . . . . .
N11 N 0.25384(7) 0.53193(7) 0.62249(6) 0.0185 1.0000 Uani . . . . . .
C12 C 0.26341(8) 0.58522(9) 0.66403(8) 0.0209 1.0000 Uani . . . . . .
C13 C 0.26958(10) 0.57305(10) 0.73350(8) 0.0280 1.0000 Uani . . . . . .
C14 C 0.26521(9) 0.65339(9) 0.64192(8) 0.0241 1.0000 Uani . . . . . .
C15 C 0.24882(9) 0.67033(9) 0.58066(8) 0.0251 1.0000 Uani . . . . . .
N16 N 0.23037(7) 0.61855(8) 0.53992(6) 0.0216 1.0000 Uani . . . . . .
B17 B 0.23591(9) 0.54513(10) 0.55681(9) 0.0198 1.0000 Uani . . . . . .
C18 C 0.22605(9) 0.48491(9) 0.50729(8) 0.0237 1.0000 Uani . . . . . .
C19 C 0.27789(11) 0.43388(10) 0.50051(9) 0.0299 1.0000 Uani . . . . . .
C20 C 0.27378(13) 0.38188(11) 0.45452(10) 0.0390 1.0000 Uani . . . . . .
C21 C 0.21633(14) 0.37902(12) 0.41508(10) 0.0453 1.0000 Uani . . . . . .
C22 C 0.16384(13) 0.42870(14) 0.42111(10) 0.0475 1.0000 Uani . . . . . .
C23 C 0.16896(10) 0.48139(12) 0.46601(9) 0.0348 1.0000 Uani . . . . . .
C24 C 0.19974(9) 0.64017(10) 0.47983(8) 0.0251 1.0000 Uani . . . . . .
C25 C 0.24012(10) 0.63893(10) 0.42533(8) 0.0290 1.0000 Uani . . . . . .
C26 C 0.31684(10) 0.61731(11) 0.42356(9) 0.0299 1.0000 Uani . . . . . .
C27 C 0.36377(11) 0.68046(13) 0.40831(11) 0.0421 1.0000 Uani . . . . . .
C28 C 0.32939(11) 0.55860(12) 0.37567(10) 0.0381 1.0000 Uani . . . . . .
C29 C 0.20779(12) 0.66017(13) 0.36962(9) 0.0409 1.0000 Uani . . . . . .
C30 C 0.13886(13) 0.68225(15) 0.36885(10) 0.0486 1.0000 Uani . . . . . .
C31 C 0.10058(11) 0.68339(13) 0.42390(10) 0.0417 1.0000 Uani . . . . . .
C32 C 0.12955(10) 0.66239(11) 0.48109(9) 0.0304 1.0000 Uani . . . . . .
C33 C 0.08513(9) 0.66347(11) 0.54068(9) 0.0355 1.0000 Uani D . . . . .
C36 C 0.25007(13) 0.74495(10) 0.55896(9) 0.0393 1.0000 Uani . . . . . .
C37 C 0.25636(9) 0.46037(9) 0.64770(7) 0.0207 1.0000 Uani . . . . . .
C38 C 0.32188(9) 0.42991(9) 0.65908(8) 0.0229 1.0000 Uani . . . . . .
C39 C 0.32269(10) 0.36418(10) 0.68804(8) 0.0280 1.0000 Uani . . . . . .
C40 C 0.26116(11) 0.33164(9) 0.70562(8) 0.0294 1.0000 Uani . . . . . .
C41 C 0.19705(10) 0.36251(10) 0.69311(8) 0.0288 1.0000 Uani . . . . . .
C42 C 0.19315(9) 0.42781(9) 0.66299(8) 0.0235 1.0000 Uani . . . . . .
C43 C 0.12248(9) 0.46076(11) 0.65006(9) 0.0310 1.0000 Uani . . . . . .
C44 C 0.08640(11) 0.48272(13) 0.71122(11) 0.0417 1.0000 Uani . . . . . .
C45 C 0.07567(11) 0.41185(14) 0.61187(11) 0.0450 1.0000 Uani . . . . . .
C46 C 0.39098(9) 0.46572(11) 0.64385(9) 0.0310 1.0000 Uani . . . . . .
C47 C 0.42999(11) 0.48524(12) 0.70429(11) 0.0421 1.0000 Uani . . . . . .
C48 C 0.43948(11) 0.41936(14) 0.60415(11) 0.0448 1.0000 Uani . . . . . .
C340 C 0.0374(5) 0.7284(4) 0.5428(5) 0.0527 0.58(2) Uani D . P 1 1 .
C341 C 0.0584(7) 0.7376(4) 0.5575(5) 0.0469 0.42(2) Uani D . P 1 2 .
C350 C 0.0240(5) 0.6123(6) 0.5415(7) 0.0457 0.42(2) Uani D . P 1 2 .
C351 C 0.0395(4) 0.5963(4) 0.5443(4) 0.0353 0.58(2) Uani D . P 1 1 .
H61 H 0.0920 0.6141 0.8289 0.0441 1.0000 Uiso R . . . . .
H71 H 0.0738 0.5695 0.9307 0.0528 1.0000 Uiso R . . . . .
H81 H -0.0254 0.6047 0.9892 0.0517 1.0000 Uiso R . . . . .
H91 H -0.1048 0.6847 0.9446 0.0553 1.0000 Uiso R . . . . .
H101 H -0.0870 0.7255 0.8416 0.0447 1.0000 Uiso R . . . . .
H132 H 0.3089 0.5995 0.7488 0.0448 1.0000 Uiso R . . . . .
H131 H 0.2754 0.5247 0.7428 0.0442 1.0000 Uiso R . . . . .
H133 H 0.2268 0.5908 0.7523 0.0450 1.0000 Uiso R . . . . .
H141 H 0.2770 0.6904 0.6689 0.0305 1.0000 Uiso R . . . . .
H191 H 0.3181 0.4358 0.5280 0.0378 1.0000 Uiso R . . . . .
H201 H 0.3107 0.3485 0.4506 0.0499 1.0000 Uiso R . . . . .
H211 H 0.2129 0.3447 0.3825 0.0549 1.0000 Uiso R . . . . .
H221 H 0.1243 0.4281 0.3939 0.0587 1.0000 Uiso R . . . . .
H231 H 0.1311 0.5157 0.4702 0.0446 1.0000 Uiso R . . . . .
H261 H 0.3299 0.6011 0.4669 0.0364 1.0000 Uiso R . . . . .
H273 H 0.4127 0.6655 0.4110 0.0635 1.0000 Uiso R . . . . .
H272 H 0.3545 0.7176 0.4386 0.0640 1.0000 Uiso R . . . . .
H271 H 0.3539 0.6965 0.3655 0.0632 1.0000 Uiso R . . . . .
H283 H 0.3785 0.5438 0.3765 0.0588 1.0000 Uiso R . . . . .
H282 H 0.3186 0.5739 0.3336 0.0580 1.0000 Uiso R . . . . .
H281 H 0.2990 0.5186 0.3852 0.0592 1.0000 Uiso R . . . . .
H291 H 0.2347 0.6580 0.3309 0.0494 1.0000 Uiso R . . . . .
H301 H 0.1172 0.6966 0.3296 0.0592 1.0000 Uiso R . . . . .
H311 H 0.0523 0.6988 0.4231 0.0523 1.0000 Uiso R . . . . .
H361 H 0.2673 0.7480 0.5161 0.0593 1.0000 Uiso R . . . . .
H363 H 0.2781 0.7723 0.5866 0.0604 1.0000 Uiso R . . . . .
H362 H 0.2037 0.7630 0.5604 0.0608 1.0000 Uiso R . . . . .
H391 H 0.3672 0.3417 0.6952 0.0360 1.0000 Uiso R . . . . .
H401 H 0.2636 0.2868 0.7262 0.0356 1.0000 Uiso R . . . . .
H411 H 0.1545 0.3399 0.7050 0.0363 1.0000 Uiso R . . . . .
H431 H 0.1293 0.5048 0.6250 0.0382 1.0000 Uiso R . . . . .
H441 H 0.0434 0.5056 0.7012 0.0645 1.0000 Uiso R . . . . .
H443 H 0.1163 0.5144 0.7372 0.0652 1.0000 Uiso R . . . . .
H442 H 0.0762 0.4403 0.7354 0.0650 1.0000 Uiso R . . . . .
H451 H 0.0325 0.4360 0.6032 0.0702 1.0000 Uiso R . . . . .
H452 H 0.0653 0.3698 0.6366 0.0708 1.0000 Uiso R . . . . .
H453 H 0.0977 0.3987 0.5717 0.0713 1.0000 Uiso R . . . . .
H461 H 0.3814 0.5099 0.6194 0.0399 1.0000 Uiso R . . . . .
H471 H 0.4749 0.5072 0.6933 0.0651 1.0000 Uiso R . . . . .
H473 H 0.4029 0.5170 0.7298 0.0661 1.0000 Uiso R . . . . .
H472 H 0.4391 0.4419 0.7280 0.0652 1.0000 Uiso R . . . . .
H481 H 0.4805 0.4468 0.5936 0.0703 1.0000 Uiso R . . . . .
H482 H 0.4539 0.3792 0.6303 0.0701 1.0000 Uiso R . . . . .
H483 H 0.4163 0.4030 0.5650 0.0707 1.0000 Uiso R . . . . .
H3401 H 0.0146 0.7310 0.5837 0.0697 0.58(2) Uiso R . P 1 1 .
H3402 H 0.0647 0.7715 0.5325 0.0698 0.58(2) Uiso R . P 1 1 .
H3403 H 0.0019 0.7193 0.5111 0.0696 0.58(2) Uiso R . P 1 1 .
H3411 H 0.0352 0.7362 0.5984 0.0711 0.42(2) Uiso R . P 1 2 .
H3412 H 0.0976 0.7701 0.5589 0.0710 0.42(2) Uiso R . P 1 2 .
H3413 H 0.0248 0.7513 0.5242 0.0719 0.42(2) Uiso R . P 1 2 .
H3502 H 0.0020 0.6156 0.5826 0.0650 0.42(2) Uiso R . P 1 2 .
H3501 H -0.0076 0.6271 0.5086 0.0651 0.42(2) Uiso R . P 1 2 .
H3503 H 0.0431 0.5657 0.5329 0.0659 0.42(2) Uiso R . P 1 2 .
H3512 H 0.0127 0.5976 0.5834 0.0532 0.58(2) Uiso R . P 1 1 .
H3511 H 0.0709 0.5555 0.5444 0.0529 0.58(2) Uiso R . P 1 1 .
H3513 H 0.0087 0.5957 0.5073 0.0533 0.58(2) Uiso R . P 1 1 .
H331 H 0.1156 0.6512 0.5742 0.0449 0.42(2) Uiso R . P 1 2 .
H332 H 0.1151 0.6652 0.5763 0.0449 0.58(2) Uiso R . P 1 1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.138(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 . B2 . 1.883(2) yes
B2 . Cl3 . 1.885(2) yes
B2 . Cl4 . 1.885(2) yes
B2 . C5 . 1.595(3) yes
C5 . C6 . 1.394(3) yes
C5 . C10 . 1.393(3) yes
C6 . C7 . 1.390(3) yes
C6 . H61 . 0.969 no
C7 . C8 . 1.381(3) yes
C7 . H71 . 0.973 no
C8 . C9 . 1.383(3) yes
C8 . H81 . 0.966 no
C9 . C10 . 1.387(3) yes
C9 . H91 . 0.968 no
C10 . H101 . 0.956 no
N11 . C12 . 1.358(2) yes
N11 . B17 . 1.459(2) yes
N11 . C37 . 1.467(2) yes
C12 . C13 . 1.498(2) yes
C12 . C14 . 1.383(2) yes
C13 . H132 . 0.962 no
C13 . H131 . 0.950 no
C13 . H133 . 0.971 no
C14 . C15 . 1.377(2) yes
C14 . H141 . 0.936 no
C15 . N16 . 1.360(2) yes
C15 . C36 . 1.496(3) yes
N16 . B17 . 1.449(2) yes
N16 . C24 . 1.464(2) yes
B17 . C18 . 1.569(2) yes
C18 . C19 . 1.397(3) yes
C18 . C23 . 1.402(3) yes
C19 . C20 . 1.394(3) yes
C19 . H191 . 0.966 no
C20 . C21 . 1.382(3) yes
C20 . H201 . 0.955 no
C21 . C22 . 1.386(4) yes
C21 . H211 . 0.955 no
C22 . C23 . 1.389(3) yes
C22 . H221 . 0.951 no
C23 . H231 . 0.979 no
C24 . C25 . 1.392(2) yes
C24 . C32 . 1.408(2) yes
C25 . C26 . 1.524(2) yes
C25 . C29 . 1.395(3) yes
C26 . C27 . 1.536(3) yes
C26 . C28 . 1.532(3) yes
C26 . H261 . 1.004 no
C27 . H273 . 0.979 no
C27 . H272 . 0.974 no
C27 . H271 . 0.978 no
C28 . H283 . 0.981 no
C28 . H282 . 0.963 no
C28 . H281 . 0.979 no
C29 . C30 . 1.384(3) yes
C29 . H291 . 0.970 no
C30 . C31 . 1.380(3) yes
C30 . H301 . 0.970 no
C31 . C32 . 1.394(3) yes
C31 . H311 . 0.969 no
C32 . C33 . 1.524(3) yes
C33 . C340 . 1.539(5) yes
C33 . C351 . 1.552(5) yes
C33 . H332 . 0.950 no
C33 . C341 . 1.546(6) yes
C33 . C350 . 1.523(6) yes
C33 . H331 . 0.950 no
C36 . H361 . 0.969 no
C36 . H363 . 0.951 no
C36 . H362 . 0.951 no
C37 . C38 . 1.402(2) yes
C37 . C42 . 1.397(2) yes
C38 . C39 . 1.396(3) yes
C38 . C46 . 1.522(2) yes
C39 . C40 . 1.381(3) yes
C39 . H391 . 0.965 no
C40 . C41 . 1.385(3) yes
C40 . H401 . 0.962 no
C41 . C42 . 1.402(3) yes
C41 . H411 . 0.954 no
C42 . C43 . 1.515(2) yes
C43 . C44 . 1.529(3) yes
C43 . C45 . 1.526(3) yes
C43 . H431 . 1.002 no
C44 . H441 . 0.956 no
C44 . H443 . 0.998 no
C44 . H442 . 0.978 no
C45 . H451 . 0.963 no
C45 . H452 . 0.978 no
C45 . H453 . 0.984 no
C46 . C47 . 1.531(3) yes
C46 . C48 . 1.534(3) yes
C46 . H461 . 1.006 no
C47 . H471 . 0.984 no
C47 . H473 . 0.964 no
C47 . H472 . 0.983 no
C48 . H481 . 0.969 no
C48 . H482 . 0.986 no
C48 . H483 . 0.993 no
C340 . H3401 . 0.974 no
C340 . H3402 . 0.999 no
C340 . H3403 . 0.971 no
C341 . H3411 . 0.976 no
C341 . H3412 . 0.974 no
C341 . H3413 . 0.988 no
C350 . H3502 . 0.971 no
C350 . H3501 . 0.965 no
C350 . H3503 . 0.978 no
C351 . H3512 . 0.976 no
C351 . H3511 . 0.983 no
C351 . H3513 . 0.983 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . B2 . Cl3 . 106.68(10) yes
Cl1 . B2 . Cl4 . 107.10(10) yes
Cl3 . B2 . Cl4 . 108.19(10) yes
Cl1 . B2 . C5 . 111.80(13) yes
Cl3 . B2 . C5 . 109.81(12) yes
Cl4 . B2 . C5 . 112.99(13) yes
B2 . C5 . C6 . 123.80(17) yes
B2 . C5 . C10 . 119.71(17) yes
C6 . C5 . C10 . 116.42(18) yes
C5 . C6 . C7 . 121.9(2) yes
C5 . C6 . H61 . 118.2 no
C7 . C6 . H61 . 119.9 no
C6 . C7 . C8 . 120.4(2) yes
C6 . C7 . H71 . 119.3 no
C8 . C7 . H71 . 120.4 no
C7 . C8 . C9 . 118.9(2) yes
C7 . C8 . H81 . 120.5 no
C9 . C8 . H81 . 120.5 no
C8 . C9 . C10 . 120.2(2) yes
C8 . C9 . H91 . 119.6 no
C10 . C9 . H91 . 120.2 no
C5 . C10 . C9 . 122.2(2) yes
C5 . C10 . H101 . 118.2 no
C9 . C10 . H101 . 119.6 no
C12 . N11 . B17 . 121.60(14) yes
C12 . N11 . C37 . 117.03(13) yes
B17 . N11 . C37 . 121.17(13) yes
N11 . C12 . C13 . 122.31(15) yes
N11 . C12 . C14 . 119.09(15) yes
C13 . C12 . C14 . 118.56(15) yes
C12 . C13 . H132 . 108.3 no
C12 . C13 . H131 . 111.4 no
H132 . C13 . H131 . 110.2 no
C12 . C13 . H133 . 106.5 no
H132 . C13 . H133 . 109.7 no
H131 . C13 . H133 . 110.5 no
C12 . C14 . C15 . 122.41(16) yes
C12 . C14 . H141 . 120.5 no
C15 . C14 . H141 . 117.1 no
C14 . C15 . N16 . 119.35(16) yes
C14 . C15 . C36 . 120.72(16) yes
N16 . C15 . C36 . 119.92(16) yes
C15 . N16 . B17 . 121.68(14) yes
C15 . N16 . C24 . 117.02(14) yes
B17 . N16 . C24 . 121.14(14) yes
N11 . B17 . N16 . 114.88(15) yes
N11 . B17 . C18 . 122.91(15) yes
N16 . B17 . C18 . 122.17(15) yes
B17 . C18 . C19 . 119.60(16) yes
B17 . C18 . C23 . 123.24(17) yes
C19 . C18 . C23 . 117.05(17) yes
C18 . C19 . C20 . 121.86(19) yes
C18 . C19 . H191 . 118.4 no
C20 . C19 . H191 . 119.7 no
C19 . C20 . C21 . 119.8(2) yes
C19 . C20 . H201 . 119.5 no
C21 . C20 . H201 . 120.6 no
C20 . C21 . C22 . 119.50(19) yes
C20 . C21 . H211 . 121.5 no
C22 . C21 . H211 . 119.0 no
C21 . C22 . C23 . 120.5(2) yes
C21 . C22 . H221 . 120.8 no
C23 . C22 . H221 . 118.7 no
C18 . C23 . C22 . 121.3(2) yes
C18 . C23 . H231 . 119.1 no
C22 . C23 . H231 . 119.6 no
N16 . C24 . C25 . 119.92(15) yes
N16 . C24 . C32 . 116.72(15) yes
C25 . C24 . C32 . 123.35(16) yes
C24 . C25 . C26 . 123.99(16) yes
C24 . C25 . C29 . 117.06(17) yes
C26 . C25 . C29 . 118.94(17) yes
C25 . C26 . C27 . 110.81(17) yes
C25 . C26 . C28 . 111.40(17) yes
C27 . C26 . C28 . 109.97(16) yes
C25 . C26 . H261 . 107.5 no
C27 . C26 . H261 . 106.8 no
C28 . C26 . H261 . 110.2 no
C26 . C27 . H273 . 108.5 no
C26 . C27 . H272 . 109.0 no
H273 . C27 . H272 . 110.2 no
C26 . C27 . H271 . 109.2 no
H273 . C27 . H271 . 109.2 no
H272 . C27 . H271 . 110.7 no
C26 . C28 . H283 . 110.4 no
C26 . C28 . H282 . 111.2 no
H283 . C28 . H282 . 108.0 no
C26 . C28 . H281 . 109.8 no
H283 . C28 . H281 . 109.9 no
H282 . C28 . H281 . 107.5 no
C25 . C29 . C30 . 121.36(19) yes
C25 . C29 . H291 . 118.1 no
C30 . C29 . H291 . 120.5 no
C29 . C30 . C31 . 120.00(19) yes
C29 . C30 . H301 . 120.1 no
C31 . C30 . H301 . 119.9 no
C30 . C31 . C32 . 121.56(18) yes
C30 . C31 . H311 . 119.7 no
C32 . C31 . H311 . 118.8 no
C24 . C32 . C31 . 116.67(17) yes
C24 . C32 . C33 . 123.43(16) yes
C31 . C32 . C33 . 119.90(17) yes
C32 . C33 . C340 . 111.4(3) yes
C32 . C33 . C351 . 110.1(4) yes
C340 . C33 . C351 . 109.17(7) yes
C32 . C33 . H332 . 109.1 no
C340 . C33 . H332 . 107.9 no
C351 . C33 . H332 . 109.1 no
C32 . C33 . C341 . 112.8(3) yes
C32 . C33 . C350 . 115.3(5) yes
C341 . C33 . C350 . 109.26(7) yes
C32 . C33 . H331 . 106.1 no
C341 . C33 . H331 . 104.9 no
C350 . C33 . H331 . 107.7 no
C15 . C36 . H361 . 110.6 no
C15 . C36 . H363 . 109.9 no
H361 . C36 . H363 . 110.9 no
C15 . C36 . H362 . 108.6 no
H361 . C36 . H362 . 108.9 no
H363 . C36 . H362 . 107.9 no
N11 . C37 . C38 . 118.54(14) yes
N11 . C37 . C42 . 118.04(15) yes
C38 . C37 . C42 . 123.28(16) yes
C37 . C38 . C39 . 117.25(16) yes
C37 . C38 . C46 . 123.58(15) yes
C39 . C38 . C46 . 119.13(16) yes
C38 . C39 . C40 . 120.86(17) yes
C38 . C39 . H391 . 118.6 no
C40 . C39 . H391 . 120.5 no
C39 . C40 . C41 . 120.71(16) yes
C39 . C40 . H401 . 118.8 no
C41 . C40 . H401 . 120.5 no
C40 . C41 . C42 . 120.80(17) yes
C40 . C41 . H411 . 120.7 no
C42 . C41 . H411 . 118.5 no
C41 . C42 . C37 . 117.06(16) yes
C41 . C42 . C43 . 119.91(16) yes
C37 . C42 . C43 . 123.01(16) yes
C42 . C43 . C44 . 111.20(16) yes
C42 . C43 . C45 . 111.45(18) yes
C44 . C43 . C45 . 110.76(17) yes
C42 . C43 . H431 . 109.2 no
C44 . C43 . H431 . 106.3 no
C45 . C43 . H431 . 107.8 no
C43 . C44 . H441 . 108.9 no
C43 . C44 . H443 . 112.1 no
H441 . C44 . H443 . 109.9 no
C43 . C44 . H442 . 108.1 no
H441 . C44 . H442 . 108.8 no
H443 . C44 . H442 . 109.0 no
C43 . C45 . H451 . 108.2 no
C43 . C45 . H452 . 109.5 no
H451 . C45 . H452 . 108.8 no
C43 . C45 . H453 . 111.5 no
H451 . C45 . H453 . 108.8 no
H452 . C45 . H453 . 110.1 no
C38 . C46 . C47 . 110.71(16) yes
C38 . C46 . C48 . 112.52(17) yes
C47 . C46 . C48 . 107.87(16) yes
C38 . C46 . H461 . 109.1 no
C47 . C46 . H461 . 108.5 no
C48 . C46 . H461 . 107.9 no
C46 . C47 . H471 . 109.2 no
C46 . C47 . H473 . 111.2 no
H471 . C47 . H473 . 109.6 no
C46 . C47 . H472 . 108.1 no
H471 . C47 . H472 . 108.9 no
H473 . C47 . H472 . 109.7 no
C46 . C48 . H481 . 107.8 no
C46 . C48 . H482 . 107.9 no
H481 . C48 . H482 . 108.9 no
C46 . C48 . H483 . 111.9 no
H481 . C48 . H483 . 109.6 no
H482 . C48 . H483 . 110.7 no
C33 . C340 . H3401 . 109.3 no
C33 . C340 . H3402 . 110.2 no
H3401 . C340 . H3402 . 112.8 no
C33 . C340 . H3403 . 104.5 no
H3401 . C340 . H3403 . 108.5 no
H3402 . C340 . H3403 . 111.1 no
C33 . C341 . H3411 . 109.2 no
C33 . C341 . H3412 . 109.5 no
H3411 . C341 . H3412 . 109.8 no
C33 . C341 . H3413 . 107.0 no
H3411 . C341 . H3413 . 110.5 no
H3412 . C341 . H3413 . 110.8 no
C33 . C350 . H3502 . 107.5 no
C33 . C350 . H3501 . 106.5 no
H3502 . C350 . H3501 . 111.1 no
C33 . C350 . H3503 . 107.1 no
H3502 . C350 . H3503 . 112.8 no
H3501 . C350 . H3503 . 111.4 no
C33 . C351 . H3512 . 108.5 no
C33 . C351 . H3511 . 108.0 no
H3512 . C351 . H3511 . 109.8 no
C33 . C351 . H3513 . 107.9 no
H3512 . C351 . H3513 . 111.6 no
H3511 . C351 . H3513 . 111.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C33 . H331 . C15 . 127.73(6) 0.950 2.576 3.245(4) yes
C33 . H332 . C15 . 129.19(6) 0.950 2.560 3.245(4) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 23/10/13 at 11:58:32
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 273,X'S) H   ( 272,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 283,X'S) H   ( 282,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 363,X'S) H   ( 362,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 443,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 473,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   ( 340,X'S) H   (3401,X'S) H   (3402,X'S) H   (3403,X'S) 
RIDE C   ( 341,X'S) H   (3411,X'S) H   (3412,X'S) H   (3413,X'S) 
RIDE C   ( 350,X'S) H   (3502,X'S) H   (3501,X'S) H   (3503,X'S) 
RIDE C   ( 351,X'S) H   (3512,X'S) H   (3511,X'S) H   (3513,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 23/10/13 at 11:58:32
#
#LIST     16                                                                    
SAME  C(33)  C(341)  C(350) AND 
CONT  C(33)  C(350)  C(341) AND 
CONT  C(33)  C(340)  C(351) AND 
CONT  C(33)  C(351)  C(340) 
SIMU 0.01 C(33)  C(341)  C(350) AND 
CONT  C(33)  C(350)  C(341) AND 
CONT  C(33)  C(340)  C(351) AND 
CONT  C(33)  C(351)  C(340) 
DELU 0.01 C(33)  C(341)  C(350) AND 
CONT  C(33)  C(350)  C(341) AND 
CONT  C(33)  C(340)  C(351) AND 
CONT  C(33)  C(351)  C(340) 
END                                                                             
;
####################################################################### 
# 
# 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_202JART14
_audit_block_doi                 10.5517/cc13vxgb
_database_code_depnum_ccdc_archive 'CCDC 1038762'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/anie.201500570 2015
_audit_update_record             
;
2014-12-11 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_audit_creation_date             2014-04-19
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '202JART14 in P -1'
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   12.5950(6)
_cell_length_b                   13.1660(4)
_cell_length_c                   18.5809(7)
_cell_angle_alpha                81.014(3)
_cell_angle_beta                 70.991(4)
_cell_angle_gamma                89.338(3)
_cell_volume                     2874.9(2)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ga -1.2846 0.7763 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135
1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C55 H40 B1 Cl2 F15 Ga1 N3 
# Dc =      1.36 Fooo =   1184.00 Mu =     22.73 M =   1179.35
# Found Formula = C52 H54 B1 Cl2 F15 Ga1 N3 
# Dc =      1.34 FOOO =   1184.00 Mu =     22.55 M =   1157.43

_chemical_formula_sum            'C52 H54 B1 Cl2 F15 Ga1 N3'
_chemical_formula_moiety         'C52 H54 B1 Cl2 F15 Ga1 N3'
_chemical_compound_source        .
_chemical_formula_weight         1157.43


_cell_measurement_reflns_used    12499
_cell_measurement_theta_min      4
_cell_measurement_theta_max      76
_cell_measurement_temperature    150

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.070
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.190

_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    2.255

# Sheldrick geometric approximatio 0.76 0.85 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.85
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            11867
_reflns_number_total             11867
_diffrn_reflns_av_R_equivalents  0.098
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11867 
# Theoretical number of reflections is about 24127 


_diffrn_reflns_theta_min         3.715
_diffrn_reflns_theta_max         76.372
_diffrn_measured_fraction_theta_max 0.983

_diffrn_reflns_theta_full        74.080
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -14
_reflns_limit_h_max              15
_reflns_limit_k_min              -16
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   2.45
_oxford_diffrn_Wilson_scale      0.05

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.90
_refine_diff_density_max         2.64


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         11820
_refine_ls_number_restraints     82
_refine_ls_number_parameters     678
_oxford_refine_ls_R_factor_ref   0.1243
_refine_ls_wR_factor_ref         0.3152
_refine_ls_goodness_of_fit_ref   0.9959
_refine_ls_shift/su_max          0.0113169
_refine_ls_shift/su_mean         0.0001908


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11820
_refine_ls_R_factor_all          0.1243
_refine_ls_wR_factor_all         0.3152

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10233
_refine_ls_R_factor_gt           0.1165
_refine_ls_wR_factor_gt          0.3071

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.18P)² +17.40P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ga1 Ga 0.22189(5) 0.78086(4) 0.34478(4) 0.0241 1.0000 Uani D . . . . .
N2 N 0.3543(3) 0.8470(3) 0.3506(2) 0.0223 1.0000 Uani . . . . . .
N53 N 0.2960(4) 0.6895(3) 0.2735(3) 0.0246 1.0000 Uani . . . . . .
N67 N 0.1921(4) 0.8948(3) 0.2632(3) 0.0328 1.0000 Uani . . . . . .
C1 C 1.083(2) 0.277(2) 0.079(3) 0.1868 0.48(3) Uani D . P 1 2 .
C2 C 1.063(3) 0.3430(17) -0.0091(15) 0.1877 0.52(3) Uani D . P 1 1 .
C3 C 0.3512(4) 0.8906(4) 0.4185(3) 0.0243 1.0000 Uani . . . . . .
C4 C 0.3638(4) 0.8243(4) 0.4826(3) 0.0263 1.0000 Uani . . . . . .
C5 C 0.3765(5) 0.7090(4) 0.4830(3) 0.0290 1.0000 Uani . . . . . .
C6 C 0.4967(5) 0.6842(4) 0.4387(4) 0.0354 1.0000 Uani . . . . . .
C7 C 0.3380(6) 0.6459(5) 0.5630(4) 0.0425 1.0000 Uani . . . . . .
C8 C 0.3636(5) 0.8671(4) 0.5464(3) 0.0336 1.0000 Uani . . . . . .
C9 C 0.3456(6) 0.9708(5) 0.5494(4) 0.0396 1.0000 Uani . . . . . .
C10 C 0.3274(5) 1.0327(4) 0.4883(4) 0.0360 1.0000 Uani . . . . . .
C11 C 0.3305(4) 0.9956(4) 0.4218(3) 0.0272 1.0000 Uani . . . . . .
C12 C 0.3068(5) 1.0670(4) 0.3571(3) 0.0312 1.0000 Uani . . . . . .
C13 C 0.3734(6) 1.1708(4) 0.3374(4) 0.0413 1.0000 Uani . . . . . .
C14 C 0.1799(6) 1.0870(5) 0.3786(4) 0.0428 1.0000 Uani . . . . . .
C15 C 0.4480(4) 0.8579(3) 0.2886(3) 0.0212 1.0000 Uani . . . . . .
C16 C 0.5460(4) 0.9257(4) 0.2876(3) 0.0226 1.0000 Uani . . . . . .
C18 C 0.7515(4) 1.0174(4) 0.2347(3) 0.0262 1.0000 Uani . . . . . .
C19 C 0.8557(5) 1.0038(4) 0.2458(3) 0.0309 1.0000 Uani . . . . . .
C21 C 0.9140(5) 1.0792(5) 0.2640(4) 0.0382 1.0000 Uani . . . . . .
C23 C 0.8728(5) 1.1766(5) 0.2680(4) 0.0390 1.0000 Uani . . . . . .
C25 C 0.7745(5) 1.1963(4) 0.2528(4) 0.0332 1.0000 Uani . . . . . .
C26 C 0.7169(4) 1.1180(4) 0.2369(3) 0.0270 1.0000 Uani . . . . . .
C29 C 0.7156(4) 0.8119(4) 0.2259(3) 0.0265 1.0000 Uani . . . . . .
C30 C 0.7264(4) 0.7447(4) 0.1734(3) 0.0298 1.0000 Uani . . . . . .
C32 C 0.7509(5) 0.6413(4) 0.1877(4) 0.0358 1.0000 Uani . . . . . .
C34 C 0.7672(5) 0.6023(4) 0.2552(4) 0.0395 1.0000 Uani . . . . . .
C36 C 0.7600(5) 0.6658(4) 0.3098(4) 0.0333 1.0000 Uani . . . . . .
C37 C 0.7345(4) 0.7676(4) 0.2936(3) 0.0281 1.0000 Uani . . . . . .
C40 C 0.6702(5) 0.9787(4) 0.1307(3) 0.0279 1.0000 Uani . . . . . .
C41 C 0.7698(5) 0.9840(4) 0.0682(4) 0.0359 1.0000 Uani . . . . . .
C43 C 0.7810(7) 1.0255(5) -0.0059(4) 0.0459 1.0000 Uani . . . . . .
C45 C 0.6879(7) 1.0680(5) -0.0231(4) 0.0466 1.0000 Uani . . . . . .
C47 C 0.5881(6) 1.0676(4) 0.0367(4) 0.0397 1.0000 Uani . . . . . .
C48 C 0.5812(5) 1.0247(4) 0.1095(3) 0.0316 1.0000 Uani . . . . . .
C51 C 0.4597(4) 0.8068(4) 0.2261(3) 0.0229 1.0000 Uani . . . . . .
C52 C 0.3965(4) 0.7224(4) 0.2211(3) 0.0253 1.0000 Uani . . . . . .
C54 C 0.2430(4) 0.5917(4) 0.2737(3) 0.0271 1.0000 Uani . . . . . .
C55 C 0.2610(5) 0.5045(4) 0.3217(3) 0.0311 1.0000 Uani . . . . . .
C56 C 0.3461(5) 0.5068(4) 0.3643(4) 0.0335 1.0000 Uani . . . . . .
C57 C 0.4619(6) 0.4748(6) 0.3145(4) 0.0472 1.0000 Uani . . . . . .
C58 C 0.3124(7) 0.4413(5) 0.4430(4) 0.0460 1.0000 Uani . . . . . .
C59 C 0.1992(5) 0.4141(4) 0.3291(4) 0.0378 1.0000 Uani . . . . . .
C60 C 0.1257(6) 0.4092(5) 0.2893(4) 0.0451 1.0000 Uani . . . . . .
C61 C 0.1128(6) 0.4930(5) 0.2395(4) 0.0432 1.0000 Uani . . . . . .
C62 C 0.1724(5) 0.5864(4) 0.2296(4) 0.0328 1.0000 Uani . . . . . .
C63 C 0.1614(5) 0.6758(5) 0.1700(4) 0.0358 1.0000 Uani . . . . . .
C64 C 0.0416(6) 0.7147(6) 0.1892(5) 0.0483 1.0000 Uani . . . . . .
C65 C 0.1989(7) 0.6477(6) 0.0892(4) 0.0486 1.0000 Uani . . . . . .
C66 C 0.4453(5) 0.6683(4) 0.1528(3) 0.0308 1.0000 Uani . . . . . .
C68 C 0.0788(5) 0.7461(4) 0.4318(4) 0.0345 1.0000 Uani D . . . . .
C69 C 0.0540(8) 0.6293(6) 0.4491(6) 0.0719 1.0000 Uani D . . . . .
C70 C -0.0190(6) 0.7975(7) 0.4098(4) 0.0543 1.0000 Uani . . . . . .
C71 C 0.0822(6) 0.7835(7) 0.5035(4) 0.0504 1.0000 Uani . . . . . .
B17 B 0.6696(5) 0.9313(4) 0.2187(3) 0.0228 1.0000 Uani . . . . . .
F20 F 0.9076(3) 0.9140(2) 0.2397(2) 0.0376 1.0000 Uani . . . . . .
F22 F 1.0116(3) 1.0586(3) 0.2774(3) 0.0581 1.0000 Uani . . . . . .
F24 F 0.9288(4) 1.2495(3) 0.2854(3) 0.0606 1.0000 Uani . . . . . .
F27 F 0.6217(3) 1.1457(2) 0.2210(2) 0.0350 1.0000 Uani . . . . . .
F28 F 0.7326(3) 1.2899(2) 0.2547(2) 0.0449 1.0000 Uani . . . . . .
F31 F 0.7102(3) 0.7743(3) 0.1054(2) 0.0371 1.0000 Uani . . . . . .
F33 F 0.7588(4) 0.5812(3) 0.1342(3) 0.0515 1.0000 Uani . . . . . .
F35 F 0.7948(4) 0.5031(3) 0.2695(3) 0.0559 1.0000 Uani . . . . . .
F38 F 0.7269(3) 0.8237(2) 0.34999(19) 0.0316 1.0000 Uani . . . . . .
F39 F 0.7782(3) 0.6296(3) 0.3757(2) 0.0467 1.0000 Uani . . . . . .
F42 F 0.8625(3) 0.9444(3) 0.0816(2) 0.0453 1.0000 Uani . . . . . .
F44 F 0.8789(4) 1.0265(4) -0.0638(2) 0.0654 1.0000 Uani . . . . . .
F46 F 0.6943(5) 1.1062(4) -0.0960(2) 0.0658 1.0000 Uani . . . . . .
F49 F 0.4787(3) 1.0298(2) 0.1642(2) 0.0351 1.0000 Uani . . . . . .
F50 F 0.4985(4) 1.1093(3) 0.0199(2) 0.0505 1.0000 Uani . . . . . .
Cl2 Cl 0.9593(8) 0.3958(4) 0.0957(4) 0.1967 1.0000 Uani D . . . . .
Cl3 Cl 0.9570(7) 0.2038(4) 0.0444(4) 0.1791 1.0000 Uani D . . . . .
H51 H 0.3279 0.6885 0.4562 0.0349 1.0000 Uiso R . . . . .
H62 H 0.5138 0.7144 0.3856 0.0526 1.0000 Uiso R . . . . .
H61 H 0.5481 0.7121 0.4597 0.0529 1.0000 Uiso R . . . . .
H63 H 0.5027 0.6112 0.4424 0.0528 1.0000 Uiso R . . . . .
H72 H 0.3466 0.5745 0.5596 0.0640 1.0000 Uiso R . . . . .
H71 H 0.3815 0.6660 0.5924 0.0639 1.0000 Uiso R . . . . .
H73 H 0.2600 0.6572 0.5879 0.0638 1.0000 Uiso R . . . . .
H81 H 0.3749 0.8248 0.5882 0.0396 1.0000 Uiso R . . . . .
H91 H 0.3457 0.9978 0.5925 0.0469 1.0000 Uiso R . . . . .
H101 H 0.3134 1.1015 0.4916 0.0431 1.0000 Uiso R . . . . .
H132 H 0.3624 1.2114 0.2930 0.0619 1.0000 Uiso R . . . . .
H131 H 0.3481 1.2081 0.3803 0.0615 1.0000 Uiso R . . . . .
H133 H 0.4526 1.1591 0.3266 0.0620 1.0000 Uiso R . . . . .
H143 H 0.1644 1.1275 0.3361 0.0640 1.0000 Uiso R . . . . .
H142 H 0.1582 1.1232 0.4219 0.0638 1.0000 Uiso R . . . . .
H141 H 0.1369 1.0229 0.3925 0.0639 1.0000 Uiso R . . . . .
H162 H 0.5202 0.9952 0.2873 0.0269 1.0000 Uiso R . . . . .
H161 H 0.5587 0.9029 0.3363 0.0272 1.0000 Uiso R . . . . .
H511 H 0.5175 0.8324 0.1811 0.0269 1.0000 Uiso R . . . . .
H561 H 0.3538 0.5784 0.3715 0.0398 1.0000 Uiso R . . . . .
H572 H 0.4550 0.4070 0.3025 0.0710 1.0000 Uiso R . . . . .
H571 H 0.4889 0.5227 0.2672 0.0710 1.0000 Uiso R . . . . .
H573 H 0.5140 0.4734 0.3424 0.0711 1.0000 Uiso R . . . . .
H582 H 0.3694 0.4476 0.4661 0.0688 1.0000 Uiso R . . . . .
H581 H 0.2441 0.4645 0.4752 0.0690 1.0000 Uiso R . . . . .
H583 H 0.3020 0.3710 0.4398 0.0690 1.0000 Uiso R . . . . .
H591 H 0.2078 0.3553 0.3618 0.0448 1.0000 Uiso R . . . . .
H601 H 0.0844 0.3482 0.2956 0.0541 1.0000 Uiso R . . . . .
H611 H 0.0643 0.4879 0.2116 0.0520 1.0000 Uiso R . . . . .
H631 H 0.2109 0.7326 0.1695 0.0428 1.0000 Uiso R . . . . .
H642 H 0.0378 0.7707 0.1503 0.0728 1.0000 Uiso R . . . . .
H641 H 0.0192 0.7372 0.2384 0.0730 1.0000 Uiso R . . . . .
H643 H -0.0087 0.6597 0.1904 0.0730 1.0000 Uiso R . . . . .
H652 H 0.1532 0.5913 0.0875 0.0728 1.0000 Uiso R . . . . .
H651 H 0.2760 0.6299 0.0750 0.0730 1.0000 Uiso R . . . . .
H653 H 0.1912 0.7052 0.0533 0.0727 1.0000 Uiso R . . . . .
H662 H 0.4055 0.6040 0.1634 0.0461 1.0000 Uiso R . . . . .
H661 H 0.5230 0.6571 0.1461 0.0458 1.0000 Uiso R . . . . .
H663 H 0.4378 0.7086 0.1076 0.0459 1.0000 Uiso R . . . . .
H693 H 0.1132 0.5960 0.4644 0.1078 1.0000 Uiso R . . . . .
H692 H -0.0158 0.6137 0.4906 0.1080 1.0000 Uiso R . . . . .
H691 H 0.0495 0.6052 0.4036 0.1078 1.0000 Uiso R . . . . .
H703 H -0.0132 0.8714 0.4069 0.0819 1.0000 Uiso R . . . . .
H702 H -0.0881 0.7714 0.4488 0.0820 1.0000 Uiso R . . . . .
H701 H -0.0192 0.7816 0.3612 0.0818 1.0000 Uiso R . . . . .
H713 H 0.1423 0.7513 0.5192 0.0758 1.0000 Uiso R . . . . .
H712 H 0.0120 0.7657 0.5444 0.0758 1.0000 Uiso R . . . . .
H711 H 0.0955 0.8570 0.4933 0.0759 1.0000 Uiso R . . . . .
H121 H 0.3285 1.0345 0.3106 0.0368 1.0000 Uiso R . . . . .
H673 H 0.1427 0.8722 0.2441 0.0490 1.0000 Uiso R . . . . .
H672 H 0.1652 0.9498 0.2842 0.0491 1.0000 Uiso R . . . . .
H671 H 0.2556 0.9136 0.2243 0.0490 1.0000 Uiso R . . . . .
H11 H 1.1541 0.2957 0.0392 0.2241 0.48(3) Uiso R . P 1 2 .
H12 H 1.0963 0.2409 0.1247 0.2240 0.48(3) Uiso R . P 1 2 .
H21 H 1.1417 0.3371 -0.0145 0.2251 0.52(3) Uiso R . P 1 1 .
H22 H 1.0552 0.3789 -0.0570 0.2251 0.52(3) Uiso R . P 1 1 .

_refine_ls_extinction_coef       60(20)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          5.0(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ga1 . N2 . 1.932(4) yes
Ga1 . N53 . 1.933(4) yes
Ga1 . N67 . 2.082(5) yes
Ga1 . C68 . 1.990(6) yes
N2 . C3 . 1.454(6) yes
N2 . C15 . 1.345(6) yes
N53 . C52 . 1.348(7) yes
N53 . C54 . 1.456(6) yes
N67 . H673 . 0.885 no
N67 . H672 . 0.888 no
N67 . H671 . 0.892 no
C1 . Cl2 . 2.180(6) yes
C1 . Cl3 . 2.173(6) yes
C1 . H11 . 0.968 no
C1 . H12 . 0.970 no
C2 . Cl2 . 2.173(6) yes
C2 . Cl3 . 2.179(6) yes
C2 . H21 . 0.970 no
C2 . H22 . 0.973 no
C3 . C4 . 1.415(8) yes
C3 . C11 . 1.410(7) yes
C4 . C5 . 1.524(7) yes
C4 . C8 . 1.388(7) yes
C5 . C6 . 1.528(7) yes
C5 . C7 . 1.513(8) yes
C5 . H51 . 0.969 no
C6 . H62 . 0.958 no
C6 . H61 . 0.960 no
C6 . H63 . 0.956 no
C7 . H72 . 0.955 no
C7 . H71 . 0.955 no
C7 . H73 . 0.961 no
C8 . C9 . 1.389(8) yes
C8 . H81 . 0.932 no
C9 . C10 . 1.371(9) yes
C9 . H91 . 0.926 no
C10 . C11 . 1.387(8) yes
C10 . H101 . 0.929 no
C11 . C12 . 1.514(8) yes
C12 . C13 . 1.541(8) yes
C12 . C14 . 1.547(8) yes
C12 . H121 . 0.982 no
C13 . H132 . 0.961 no
C13 . H131 . 0.965 no
C13 . H133 . 0.967 no
C14 . H143 . 0.955 no
C14 . H142 . 0.960 no
C14 . H141 . 0.961 no
C15 . C16 . 1.524(6) yes
C15 . C51 . 1.397(7) yes
C16 . B17 . 1.656(7) yes
C16 . H162 . 0.968 no
C16 . H161 . 0.970 no
C18 . C19 . 1.399(7) yes
C18 . C26 . 1.392(7) yes
C18 . B17 . 1.664(7) yes
C19 . C21 . 1.386(8) yes
C19 . F20 . 1.347(6) yes
C21 . C23 . 1.381(9) yes
C21 . F22 . 1.348(7) yes
C23 . C25 . 1.370(9) yes
C23 . F24 . 1.337(7) yes
C25 . C26 . 1.388(7) yes
C25 . F28 . 1.337(6) yes
C26 . F27 . 1.359(6) yes
C29 . C30 . 1.390(7) yes
C29 . C37 . 1.395(8) yes
C29 . B17 . 1.669(7) yes
C30 . C32 . 1.397(8) yes
C30 . F31 . 1.341(7) yes
C32 . C34 . 1.357(10) yes
C32 . F33 . 1.344(7) yes
C34 . C36 . 1.393(9) yes
C34 . F35 . 1.356(7) yes
C36 . C37 . 1.384(7) yes
C36 . F39 . 1.333(7) yes
C37 . F38 . 1.351(6) yes
C40 . C41 . 1.398(8) yes
C40 . C48 . 1.405(8) yes
C40 . B17 . 1.656(8) yes
C41 . C43 . 1.361(9) yes
C41 . F42 . 1.353(8) yes
C43 . C45 . 1.401(12) yes
C43 . F44 . 1.345(8) yes
C45 . C47 . 1.380(11) yes
C45 . F46 . 1.346(8) yes
C47 . C48 . 1.357(9) yes
C47 . F50 . 1.355(8) yes
C48 . F49 . 1.367(7) yes
C51 . C52 . 1.407(7) yes
C51 . H511 . 0.929 no
C52 . C66 . 1.503(7) yes
C54 . C55 . 1.403(8) yes
C54 . C62 . 1.402(8) yes
C55 . C56 . 1.528(8) yes
C55 . C59 . 1.394(7) yes
C56 . C57 . 1.546(9) yes
C56 . C58 . 1.508(9) yes
C56 . H561 . 0.983 no
C57 . H572 . 0.965 no
C57 . H571 . 0.960 no
C57 . H573 . 0.958 no
C58 . H582 . 0.959 no
C58 . H581 . 0.951 no
C58 . H583 . 0.950 no
C59 . C60 . 1.367(10) yes
C59 . H591 . 0.934 no
C60 . C61 . 1.369(10) yes
C60 . H601 . 0.933 no
C61 . C62 . 1.404(8) yes
C61 . H611 . 0.929 no
C62 . C63 . 1.523(9) yes
C63 . C64 . 1.535(9) yes
C63 . C65 . 1.524(9) yes
C63 . H631 . 0.976 no
C64 . H642 . 0.961 no
C64 . H641 . 0.958 no
C64 . H643 . 0.960 no
C65 . H652 . 0.955 no
C65 . H651 . 0.957 no
C65 . H653 . 0.953 no
C66 . H662 . 0.948 no
C66 . H661 . 0.958 no
C66 . H663 . 0.953 no
C68 . C69 . 1.535(9) yes
C68 . C70 . 1.538(10) yes
C68 . C71 . 1.503(10) yes
C69 . H693 . 0.959 no
C69 . H692 . 0.961 no
C69 . H691 . 0.967 no
C70 . H703 . 0.968 no
C70 . H702 . 0.959 no
C70 . H701 . 0.959 no
C71 . H713 . 0.968 no
C71 . H712 . 0.962 no
C71 . H711 . 0.962 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 . Ga1 . N53 . 98.25(17) yes
N2 . Ga1 . N67 . 96.80(18) yes
N53 . Ga1 . N67 . 96.43(19) yes
N2 . Ga1 . C68 . 125.4(2) yes
N53 . Ga1 . C68 . 124.8(2) yes
N67 . Ga1 . C68 . 108.4(2) yes
Ga1 . N2 . C3 . 121.0(3) yes
Ga1 . N2 . C15 . 118.6(3) yes
C3 . N2 . C15 . 120.2(4) yes
Ga1 . N53 . C52 . 117.2(3) yes
Ga1 . N53 . C54 . 121.5(3) yes
C52 . N53 . C54 . 121.3(4) yes
Ga1 . N67 . H673 . 110.8 no
Ga1 . N67 . H672 . 110.6 no
H673 . N67 . H672 . 108.2 no
Ga1 . N67 . H671 . 110.3 no
H673 . N67 . H671 . 108.1 no
H672 . N67 . H671 . 108.6 no
Cl2 . C1 . Cl3 . 81.49(7) yes
Cl2 . C1 . H11 . 115.9 no
Cl3 . C1 . H11 . 116.1 no
Cl2 . C1 . H12 . 116.9 no
Cl3 . C1 . H12 . 115.9 no
H11 . C1 . H12 . 108.7 no
Cl2 . C2 . Cl3 . 81.52(7) yes
Cl2 . C2 . H21 . 115.2 no
Cl3 . C2 . H21 . 115.8 no
Cl2 . C2 . H22 . 115.9 no
Cl3 . C2 . H22 . 116.5 no
H21 . C2 . H22 . 109.7 no
N2 . C3 . C4 . 118.5(4) yes
N2 . C3 . C11 . 120.8(5) yes
C4 . C3 . C11 . 120.7(5) yes
C3 . C4 . C5 . 121.7(5) yes
C3 . C4 . C8 . 118.1(5) yes
C5 . C4 . C8 . 120.2(5) yes
C4 . C5 . C6 . 111.7(4) yes
C4 . C5 . C7 . 113.6(5) yes
C6 . C5 . C7 . 110.4(5) yes
C4 . C5 . H51 . 106.1 no
C6 . C5 . H51 . 107.8 no
C7 . C5 . H51 . 107.0 no
C5 . C6 . H62 . 108.6 no
C5 . C6 . H61 . 109.7 no
H62 . C6 . H61 . 109.6 no
C5 . C6 . H63 . 109.6 no
H62 . C6 . H63 . 109.2 no
H61 . C6 . H63 . 110.1 no
C5 . C7 . H72 . 109.9 no
C5 . C7 . H71 . 109.8 no
H72 . C7 . H71 . 109.5 no
C5 . C7 . H73 . 109.1 no
H72 . C7 . H73 . 109.0 no
H71 . C7 . H73 . 109.6 no
C4 . C8 . C9 . 121.4(5) yes
C4 . C8 . H81 . 119.1 no
C9 . C8 . H81 . 119.5 no
C8 . C9 . C10 . 119.5(5) yes
C8 . C9 . H91 . 120.0 no
C10 . C9 . H91 . 120.4 no
C9 . C10 . C11 . 121.9(5) yes
C9 . C10 . H101 . 118.7 no
C11 . C10 . H101 . 119.4 no
C3 . C11 . C10 . 118.2(5) yes
C3 . C11 . C12 . 122.3(5) yes
C10 . C11 . C12 . 119.5(5) yes
C11 . C12 . C13 . 112.0(5) yes
C11 . C12 . C14 . 110.5(5) yes
C13 . C12 . C14 . 109.1(5) yes
C11 . C12 . H121 . 109.2 no
C13 . C12 . H121 . 108.1 no
C14 . C12 . H121 . 107.8 no
C12 . C13 . H132 . 109.9 no
C12 . C13 . H131 . 110.1 no
H132 . C13 . H131 . 108.9 no
C12 . C13 . H133 . 109.9 no
H132 . C13 . H133 . 109.2 no
H131 . C13 . H133 . 108.8 no
C12 . C14 . H143 . 110.3 no
C12 . C14 . H142 . 109.0 no
H143 . C14 . H142 . 109.4 no
C12 . C14 . H141 . 110.2 no
H143 . C14 . H141 . 109.1 no
H142 . C14 . H141 . 108.9 no
N2 . C15 . C16 . 118.8(4) yes
N2 . C15 . C51 . 122.1(4) yes
C16 . C15 . C51 . 119.0(4) yes
C15 . C16 . B17 . 121.7(4) yes
C15 . C16 . H162 . 106.6 no
B17 . C16 . H162 . 106.9 no
C15 . C16 . H161 . 105.7 no
B17 . C16 . H161 . 107.1 no
H162 . C16 . H161 . 108.3 no
C19 . C18 . C26 . 112.6(5) yes
C19 . C18 . B17 . 128.6(4) yes
C26 . C18 . B17 . 118.8(4) yes
C18 . C19 . C21 . 124.0(5) yes
C18 . C19 . F20 . 121.6(5) yes
C21 . C19 . F20 . 114.4(5) yes
C19 . C21 . C23 . 120.1(5) yes
C19 . C21 . F22 . 120.4(5) yes
C23 . C21 . F22 . 119.4(5) yes
C21 . C23 . C25 . 118.3(5) yes
C21 . C23 . F24 . 120.3(6) yes
C25 . C23 . F24 . 121.4(5) yes
C23 . C25 . C26 . 119.8(5) yes
C23 . C25 . F28 . 120.3(5) yes
C26 . C25 . F28 . 119.8(5) yes
C18 . C26 . C25 . 124.8(5) yes
C18 . C26 . F27 . 119.8(4) yes
C25 . C26 . F27 . 115.4(4) yes
C30 . C29 . C37 . 113.9(5) yes
C30 . C29 . B17 . 126.3(5) yes
C37 . C29 . B17 . 119.3(4) yes
C29 . C30 . C32 . 123.3(6) yes
C29 . C30 . F31 . 121.9(5) yes
C32 . C30 . F31 . 114.8(5) yes
C30 . C32 . C34 . 120.0(5) yes
C30 . C32 . F33 . 119.5(6) yes
C34 . C32 . F33 . 120.5(5) yes
C32 . C34 . C36 . 119.8(5) yes
C32 . C34 . F35 . 121.2(6) yes
C36 . C34 . F35 . 118.9(6) yes
C34 . C36 . C37 . 118.4(6) yes
C34 . C36 . F39 . 120.7(5) yes
C37 . C36 . F39 . 120.9(5) yes
C29 . C37 . C36 . 124.6(5) yes
C29 . C37 . F38 . 120.6(4) yes
C36 . C37 . F38 . 114.8(5) yes
C41 . C40 . C48 . 112.5(5) yes
C41 . C40 . B17 . 120.0(5) yes
C48 . C40 . B17 . 127.3(5) yes
C40 . C41 . C43 . 124.9(6) yes
C40 . C41 . F42 . 118.1(5) yes
C43 . C41 . F42 . 117.0(6) yes
C41 . C43 . C45 . 119.5(6) yes
C41 . C43 . F44 . 122.1(7) yes
C45 . C43 . F44 . 118.4(6) yes
C43 . C45 . C47 . 118.1(6) yes
C43 . C45 . F46 . 121.3(7) yes
C47 . C45 . F46 . 120.6(7) yes
C45 . C47 . C48 . 120.1(6) yes
C45 . C47 . F50 . 118.0(6) yes
C48 . C47 . F50 . 121.9(6) yes
C40 . C48 . C47 . 124.8(6) yes
C40 . C48 . F49 . 120.1(5) yes
C47 . C48 . F49 . 115.0(5) yes
C15 . C51 . C52 . 129.5(5) yes
C15 . C51 . H511 . 115.4 no
C52 . C51 . H511 . 115.1 no
C51 . C52 . N53 . 123.3(4) yes
C51 . C52 . C66 . 117.0(4) yes
N53 . C52 . C66 . 119.7(4) yes
N53 . C54 . C55 . 118.1(5) yes
N53 . C54 . C62 . 120.5(5) yes
C55 . C54 . C62 . 121.3(5) yes
C54 . C55 . C56 . 121.8(5) yes
C54 . C55 . C59 . 117.9(5) yes
C56 . C55 . C59 . 120.3(5) yes
C55 . C56 . C57 . 110.1(5) yes
C55 . C56 . C58 . 114.8(5) yes
C57 . C56 . C58 . 109.3(5) yes
C55 . C56 . H561 . 107.0 no
C57 . C56 . H561 . 108.2 no
C58 . C56 . H561 . 107.1 no
C56 . C57 . H572 . 109.7 no
C56 . C57 . H571 . 109.6 no
H572 . C57 . H571 . 108.9 no
C56 . C57 . H573 . 109.7 no
H572 . C57 . H573 . 108.8 no
H571 . C57 . H573 . 110.1 no
C56 . C58 . H582 . 109.7 no
C56 . C58 . H581 . 109.6 no
H582 . C58 . H581 . 108.3 no
C56 . C58 . H583 . 110.9 no
H582 . C58 . H583 . 109.2 no
H581 . C58 . H583 . 109.0 no
C55 . C59 . C60 . 121.3(6) yes
C55 . C59 . H591 . 119.8 no
C60 . C59 . H591 . 118.9 no
C59 . C60 . C61 . 120.6(5) yes
C59 . C60 . H601 . 120.0 no
C61 . C60 . H601 . 119.4 no
C60 . C61 . C62 . 120.8(6) yes
C60 . C61 . H611 . 119.7 no
C62 . C61 . H611 . 119.4 no
C61 . C62 . C54 . 117.9(6) yes
C61 . C62 . C63 . 119.3(6) yes
C54 . C62 . C63 . 122.8(5) yes
C62 . C63 . C64 . 112.7(5) yes
C62 . C63 . C65 . 111.5(5) yes
C64 . C63 . C65 . 109.4(6) yes
C62 . C63 . H631 . 107.9 no
C64 . C63 . H631 . 107.6 no
C65 . C63 . H631 . 107.5 no
C63 . C64 . H642 . 110.3 no
C63 . C64 . H641 . 110.0 no
H642 . C64 . H641 . 109.6 no
C63 . C64 . H643 . 109.0 no
H642 . C64 . H643 . 108.4 no
H641 . C64 . H643 . 109.6 no
C63 . C65 . H652 . 110.2 no
C63 . C65 . H651 . 109.7 no
H652 . C65 . H651 . 109.9 no
C63 . C65 . H653 . 109.5 no
H652 . C65 . H653 . 108.6 no
H651 . C65 . H653 . 108.9 no
C52 . C66 . H662 . 107.8 no
C52 . C66 . H661 . 109.0 no
H662 . C66 . H661 . 109.6 no
C52 . C66 . H663 . 110.2 no
H662 . C66 . H663 . 110.1 no
H661 . C66 . H663 . 110.1 no
Ga1 . C68 . C69 . 110.2(4) yes
Ga1 . C68 . C70 . 109.7(4) yes
C69 . C68 . C70 . 107.8(7) yes
Ga1 . C68 . C71 . 111.8(4) yes
C69 . C68 . C71 . 109.5(7) yes
C70 . C68 . C71 . 107.7(5) yes
C68 . C69 . H693 . 109.1 no
C68 . C69 . H692 . 109.3 no
H693 . C69 . H692 . 109.0 no
C68 . C69 . H691 . 109.9 no
H693 . C69 . H691 . 109.7 no
H692 . C69 . H691 . 109.8 no
C68 . C70 . H703 . 110.5 no
C68 . C70 . H702 . 108.4 no
H703 . C70 . H702 . 108.9 no
C68 . C70 . H701 . 110.4 no
H703 . C70 . H701 . 109.7 no
H702 . C70 . H701 . 109.0 no
C68 . C71 . H713 . 109.5 no
C68 . C71 . H712 . 109.8 no
H713 . C71 . H712 . 108.9 no
C68 . C71 . H711 . 109.8 no
H713 . C71 . H711 . 109.1 no
H712 . C71 . H711 . 109.7 no
C29 . B17 . C18 . 113.5(4) yes
C29 . B17 . C16 . 105.3(4) yes
C18 . B17 . C16 . 107.5(4) yes
C29 . B17 . C40 . 113.1(4) yes
C18 . B17 . C40 . 102.0(4) yes
C16 . B17 . C40 . 115.6(4) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C51 . H511 . C40 . 139.09 0.929 2.576 3.334(10) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 19/04/14 at 15:11:57
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
CONT EXTPARAM 
RIDE N   (  67,X'S) H   ( 673,X'S) H   ( 672,X'S) H   ( 671,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  62,X'S) H   (  61,X'S) H   (  63,X'S) 
RIDE C   (   7,X'S) H   (  72,X'S) H   (  71,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 572,X'S) H   ( 571,X'S) H   ( 573,X'S) 
RIDE C   (  58,X'S) H   ( 582,X'S) H   ( 581,X'S) H   ( 583,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 642,X'S) H   ( 641,X'S) H   ( 643,X'S) 
RIDE C   (  65,X'S) H   ( 652,X'S) H   ( 651,X'S) H   ( 653,X'S) 
RIDE C   (  66,X'S) H   ( 662,X'S) H   ( 661,X'S) H   ( 663,X'S) 
RIDE C   (  69,X'S) H   ( 693,X'S) H   ( 692,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 703,X'S) H   ( 702,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 713,X'S) H   ( 712,X'S) H   ( 711,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 19/04/14 at 15:11:57
#
#LIST     16                                                                    
REM 
REM DICHLOROMETHANE 
REM 
SAME  C(1)  CL(3)  CL(2) AND 
CONT  C(1)  CL(2)  CL(3) AND 
CONT  C(2)  CL(3)  CL(2) AND 
CONT  C(2)  CL(2)  CL(3) 
SIMU 0.01 C(1)  CL(3)  CL(2) AND 
CONT  C(1)  CL(2)  CL(3) AND 
CONT  C(2)  CL(3)  CL(2) AND 
CONT  C(2)  CL(2)  CL(3) 
DELU 0.01 C(1)  CL(3)  CL(2) AND 
CONT  C(1)  CL(2)  CL(3) AND 
CONT  C(2)  CL(3)  CL(2) AND 
CONT  C(2)  CL(2)  CL(3) 
SIMU 0.01  GA(1)  C(68)  C(69) 
DELU 0.01  GA(1)  C(68)  C(69) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.094 0.539 0.604 8 0 ' '
2 0.500 0.500 0.000 352 83 ' '
3 0.906 0.460 0.396 8 0 ' '
_platon_squeeze_details          
;
;
