# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_Ni42_Cl2
_database_code_depnum_ccdc_archive 'CCDC 1533111'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
_audit_creation_date             2017-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C64 H38 F34 N8 Ni O2, 2(Cl), 2(C2 H6 O S), H2 O'
_chemical_formula_sum            'C68 H52 Cl2 F34 N8 Ni O5 S2'
_chemical_formula_weight         1900.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.4507(7)
_cell_length_b                   13.2384(8)
_cell_length_c                   26.961(2)
_cell_angle_alpha                95.396(6)
_cell_angle_beta                 91.534(6)
_cell_angle_gamma                90.814(5)
_cell_volume                     3711.7(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3482
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.4820
_cell_measurement_theta_min      3.5710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77879
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 5 7 0.0313
3 -7 -5 0.0529
-5 -5 5 0.0328
6 3 -7 0.0363
1 -2 17 0.0135
-1 2 -17 0.0203
6 0 -6 0.0297

_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.034
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.9999 5.0000 6.9976 -0.1913 -0.5969 0.6911
2.9999 -7.0000 -4.9969 0.1870 0.8239 -0.5089
-5.0001 -4.9999 5.0014 0.1519 0.5463 0.7856
6.0001 2.9999 -7.0005 -0.0780 -0.3109 -0.9636
0.9998 -1.9999 17.0003 -0.9162 0.2762 0.2782
-0.9998 1.9999 -17.0003 0.9162 -0.2762 -0.2782
6.0000 -0.0000 -5.9994 -0.0779 0.0380 -0.9365

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.1108
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20793
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.746
_diffrn_reflns_theta_max         66.746
_diffrn_reflns_theta_min         3.354
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00 -17.00   1.50   21.00    --  -41.90 -37.00   0.00   60
  2  ω    -66.00  28.50   1.50   21.00    --  -41.90  37.00-180.00   63
  3  ω    -96.00  -6.00   1.50   21.00    --  -41.90 125.00 -90.00   60
  4  ω    -96.00  -3.00   1.50   21.00    --  -41.90 125.00-180.00   62
  5  ω     44.00 135.50   1.50   84.00    --  112.00 -77.00  30.00   61
  6  ω     88.00 178.00   1.50   84.00    --  112.00  45.00  90.00   60
  7  ω     58.00 136.00   1.50   84.00    --  112.00 -30.00  30.00   52
  8  ω     93.00 174.00   1.50   84.00    --  112.00  30.00-150.00   54
  9  ω     43.00 115.00   1.50   84.00    --  112.00-111.00-150.00   48
 10  ω     38.00 122.00   1.50   84.00    --  112.00 -89.00 -59.00   56
 11  ω     51.00 135.00   1.50   84.00    --  112.00 -45.00 150.00   56
 12  ω     39.00 117.00   1.50   84.00    --  112.00 -30.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0650949000
_diffrn_orient_matrix_UB_12      -0.0174057000
_diffrn_orient_matrix_UB_13      -0.0521106000
_diffrn_orient_matrix_UB_21      0.0084789000
_diffrn_orient_matrix_UB_22      -0.1155978000
_diffrn_orient_matrix_UB_23      0.0021465000
_diffrn_orient_matrix_UB_31      -0.1320712000
_diffrn_orient_matrix_UB_32      -0.0010368000
_diffrn_orient_matrix_UB_33      0.0240112000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8000
_reflns_number_total             13059
_reflns_odcompleteness_completeness 99.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.941
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         13059
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0792
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1066P)²+2.4553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2330
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) = Uanis(C29)
Uanis(C25) = Uanis(C24)
3. Others
 Sof(F3)=Sof(F4)=Sof(F7)=Sof(F8)=Sof(H23C)=Sof(H23D)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(C26)=Sof(C29)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F5)=Sof(F6)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(C27)=Sof(C28)=FVAR(1)
 Fixed Sof: S1(0.5) S2(0.5) F22(0.5) F23(0.5) F24(0.5) F25(0.5) F26(0.5)
 F27(0.5) F28(0.5) F29(0.5) F30(0.5) F31(0.5) F32(0.5) F33(0.5) F34(0.5)
 F35(0.5) F36(0.5) F37(0.5) F38(0.5) F39(0.5) F40(0.5) F41(0.5) F42(0.5)
 F43(0.5) F44(0.5) F45(0.5) F46(0.5) F47(0.5) F48(0.5) F49(0.5) F50(0.5)
 F51(0.5) F52(0.5) F53(0.5) F54(0.5) F55(0.5) C67(0.5) C68(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) H71D(0.5) H71E(0.5) H71F(0.5) C72(0.5) H72A(0.5) H72B(0.5)
 H72C(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5)
4.a Riding coordinates:
 O5(H5A,H5B), N7(H7), N8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C23(H23C,H23D), C24(H24A,H24B), C25(H25A,H25B), C58(H58A,
 H58B), C59(H59A,H59B)
4.c Me refined with riding coordinates:
 C71(H71A,H71B,H71C), C71(H71D,H71E,H71F)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7A), C9(H9), C12(H12), C13(H13), C14(H14),
  C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C36(H36), C37(H37),
 C38(H38), C39(H39), C42(H42), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50),
  C52(H52), C53(H53), C55(H55), C56(H56)
4.e Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.43062(8) 0.72185(6) 0.63247(3) 0.0225(2) Uani 1 1 d . . . . .
Cl1 Cl 0.87804(13) 0.31113(10) 0.57762(5) 0.0319(3) Uani 1 1 d . . . . .
Cl2 Cl 1.07924(14) 0.01127(10) 0.71862(5) 0.0340(3) Uani 1 1 d . . . . .
S1 S 0.2942(3) 0.2829(2) 0.66356(12) 0.0349(6) Uani 0.5 1 d . . P A 2
S2 S 0.3263(3) 0.2067(3) 0.63950(13) 0.0449(8) Uani 0.5 1 d . . P A 1
S3 S 0.5946(3) 0.8936(2) 0.80450(12) 0.0839(8) Uani 1 1 d . . . . .
F1 F 0.0135(7) 1.2909(5) 0.1938(3) 0.0523(17) Uani 0.674(7) 1 d . . P B 1
F2 F 0.1706(7) 1.4020(7) 0.1979(3) 0.066(2) Uani 0.674(7) 1 d . . P B 1
F3 F -0.0576(19) 1.3248(9) 0.2082(5) 0.059(4) Uani 0.326(7) 1 d . . P B 2
F4 F 0.115(2) 1.4220(15) 0.2221(6) 0.064(5) Uani 0.326(7) 1 d . . P B 2
F5 F -0.1413(5) 1.4188(5) 0.2417(2) 0.0416(15) Uani 0.674(7) 1 d . . P B 1
F6 F 0.0137(8) 1.5235(6) 0.2674(2) 0.0529(18) Uani 0.674(7) 1 d . . P B 1
F7 F -0.0469(14) 1.5685(9) 0.2690(4) 0.041(3) Uani 0.326(7) 1 d . . P B 2
F8 F -0.2113(14) 1.4692(10) 0.2461(5) 0.048(3) Uani 0.326(7) 1 d . . P B 2
F9 F -0.0612(6) 1.4508(3) 0.14341(16) 0.0701(15) Uani 1 1 d . . . . .
F10 F 0.0447(5) 1.5822(4) 0.17975(17) 0.0678(14) Uani 1 1 d . . . . .
F11 F -0.1995(7) 1.6349(6) 0.2240(2) 0.113(3) Uani 1 1 d . . . . .
F12 F -0.2785(6) 1.5219(5) 0.1671(2) 0.0866(18) Uani 1 1 d . . . . .
F13 F -0.1147(5) 1.6232(3) 0.10031(17) 0.0622(13) Uani 1 1 d . . . . .
F14 F -0.1000(5) 1.7437(4) 0.1610(2) 0.0777(16) Uani 1 1 d . . . . .
F15 F -0.3755(6) 1.7166(5) 0.1641(3) 0.097(2) Uani 1 1 d . . . . .
F16 F -0.3594(5) 1.6317(4) 0.0910(2) 0.0760(15) Uani 1 1 d . . . . .
F17 F -0.2804(6) 1.8805(4) 0.1347(3) 0.104(2) Uani 1 1 d . . . . .
F18 F -0.1941(5) 1.8020(4) 0.0688(3) 0.0816(18) Uani 1 1 d . . . . .
F19 F -0.4219(6) 1.7663(5) 0.0245(3) 0.095(2) Uani 1 1 d . . . . .
F20 F -0.4047(6) 1.9214(5) 0.0546(4) 0.120(3) Uani 1 1 d . . . . .
F21 F -0.5186(6) 1.8163(5) 0.0916(3) 0.116(3) Uani 1 1 d . . . . .
F22 F 1.1150(8) -0.0171(6) 0.9448(3) 0.0483(19) Uani 0.5 1 d . . P C 1
F23 F 1.1747(12) -0.0811(10) 0.8931(4) 0.059(3) Uani 0.5 1 d . . P C 2
F24 F 1.1356(10) -0.1274(7) 0.8796(4) 0.038(2) Uani 0.5 1 d . . P C 1
F25 F 1.0196(11) -0.1879(7) 0.8713(3) 0.068(3) Uani 0.5 1 d . . P C 2
F26 F 0.9512(7) -0.2495(6) 0.9218(3) 0.0440(18) Uani 0.5 1 d . . P D 1
F27 F 0.942(4) -0.153(3) 0.9744(13) 0.057(7) Uani 0.5 1 d . . P D 2
F28 F 0.966(4) -0.147(3) 0.9879(13) 0.062(7) Uani 0.5 1 d . . P D 1
F29 F 1.1257(9) -0.0795(6) 0.9868(3) 0.053(2) Uani 0.5 1 d . . P D 2
F30 F 1.2398(8) -0.1699(6) 0.9812(4) 0.059(2) Uani 0.5 1 d . . P E 1
F31 F 1.2282(17) -0.2525(10) 0.9289(7) 0.054(4) Uani 0.5 1 d . . P E 2
F32 F 1.1921(15) -0.2913(10) 0.9232(6) 0.044(3) Uani 0.5 1 d . . P E 1
F33 F 1.0402(9) -0.3244(6) 0.9383(3) 0.056(2) Uani 0.5 1 d . . P E 2
F34 F 1.0094(7) -0.3546(7) 0.9976(3) 0.051(2) Uani 0.5 1 d . . P F 1
F35 F 1.0770(13) -0.2528(16) 1.0422(7) 0.043(3) Uani 0.5 1 d . . P F 2
F36 F 1.1265(14) -0.2554(16) 1.0488(7) 0.049(4) Uani 0.5 1 d . . P F 1
F37 F 1.2764(8) -0.2263(6) 1.0227(3) 0.051(2) Uani 0.5 1 d . . P F 2
F38 F 1.3424(8) -0.3515(7) 1.0022(4) 0.060(2) Uani 0.5 1 d . . P G 1
F39 F 1.2529(16) -0.4285(10) 0.9683(6) 0.057(4) Uani 0.5 1 d . . P G 2
F40 F 1.2052(15) -0.4617(10) 0.9674(6) 0.047(3) Uani 0.5 1 d . . P G 1
F41 F 1.0820(8) -0.4432(6) 1.0143(4) 0.056(2) Uani 0.5 1 d . . P G 2
F42 F 1.1091(9) -0.4707(7) 1.0664(4) 0.060(2) Uani 0.5 1 d . . P H 1
F43 F 1.2478(19) -0.3664(14) 1.0965(8) 0.050(4) Uani 0.5 1 d . . P H 2
F44 F 1.288(2) -0.3900(17) 1.0896(9) 0.071(5) Uani 0.5 1 d . . P H 1
F45 F 1.4027(8) -0.3963(7) 1.0447(4) 0.059(2) Uani 0.5 1 d . . P H 2
F46 F 1.4073(11) -0.5408(9) 1.0243(4) 0.078(3) Uani 0.5 1 d . . P I 1
F47 F 1.2803(16) -0.5906(12) 1.0200(7) 0.056(4) Uani 0.5 1 d . . P I 2
F48 F 1.2302(19) -0.6192(14) 1.0218(8) 0.069(5) Uani 0.5 1 d . . P I 1
F49 F 1.1709(8) -0.5542(7) 1.0875(3) 0.052(2) Uani 0.5 1 d . . P I 2
F50 F 1.2333(16) -0.6057(13) 1.1232(6) 0.124(6) Uani 0.5 1 d . . P I 1
F51 F 1.385(3) -0.6869(16) 1.0879(8) 0.122(9) Uani 0.5 1 d . . P I 1
F52 F 1.3675(17) -0.6590(12) 1.1103(6) 0.071(4) Uani 0.5 1 d . . P I 2
F53 F 1.4973(9) -0.5723(8) 1.0703(4) 0.069(3) Uani 0.5 1 d . . P I 2
F54 F 1.420(2) -0.5473(13) 1.1214(10) 0.108(8) Uani 0.5 1 d . . P I 1
F55 F 1.4098(18) -0.5066(9) 1.1358(5) 0.059(3) Uani 0.5 1 d . . P I 2
O1 O 0.1688(4) 1.3075(3) 0.37176(16) 0.0345(9) Uani 1 1 d . . . . .
O2 O 0.7826(5) 0.1148(3) 0.86836(17) 0.0443(11) Uani 1 1 d . . . . .
O3 O 0.3895(5) 0.3139(5) 0.6293(2) 0.0591(14) Uani 1 1 d . . . . .
O4 O 0.7278(7) 0.8929(5) 0.7999(3) 0.088(2) Uani 1 1 d . . . . .
O5 O 0.5875(5) 0.2243(3) 0.56652(19) 0.0468(11) Uani 1 1 d . . . . .
H5A H 0.5373 0.2497 0.5877 0.070 Uiso 1 1 d R . . . .
H5B H 0.6637 0.2440 0.5709 0.070 Uiso 1 1 d R . . . .
N1 N 0.5486(4) 0.8527(3) 0.64418(17) 0.0251(9) Uani 1 1 d . . . . .
N2 N 0.3403(4) 0.8190(3) 0.59156(16) 0.0229(9) Uani 1 1 d . . . . .
N3 N 0.2619(4) 0.6402(3) 0.60863(17) 0.0247(9) Uani 1 1 d . . . . .
N4 N 0.5344(4) 0.6507(3) 0.57248(17) 0.0245(9) Uani 1 1 d . . . . .
N5 N 0.5218(4) 0.6129(3) 0.66509(17) 0.0240(9) Uani 1 1 d . . . . .
N6 N 0.3728(4) 0.7468(3) 0.70730(17) 0.0260(9) Uani 1 1 d . . . . .
N7 N 0.0475(5) 1.1601(3) 0.36507(18) 0.0296(10) Uani 1 1 d . . . . .
H7 H 0.0017 1.1107 0.3406 0.08(3) Uiso 1 1 d R . . . .
N8 N 0.8763(5) 0.1241(4) 0.79364(19) 0.0348(11) Uani 1 1 d . . . . .
H8 H 0.9403 0.0890 0.7720 0.042 Uiso 1 1 d R . . J 1
C1 C 0.2242(5) 0.5488(4) 0.6213(2) 0.0282(11) Uani 1 1 d . . . . .
H1 H 0.2759 0.5161 0.6432 0.034 Uiso 1 1 calc R . . . .
C2 C 0.1118(6) 0.5016(4) 0.6030(2) 0.0298(12) Uani 1 1 d . . . . .
H2 H 0.0870 0.4392 0.6132 0.036 Uiso 1 1 calc R . . . .
C3 C 0.0371(5) 0.5479(4) 0.5695(2) 0.0292(12) Uani 1 1 d . . . . .
H3 H -0.0385 0.5168 0.5565 0.035 Uiso 1 1 calc R . . . .
C4 C 0.0750(5) 0.6413(4) 0.5552(2) 0.0259(11) Uani 1 1 d . . . . .
H4 H 0.0263 0.6730 0.5320 0.031 Uiso 1 1 calc R . . . .
C5 C 0.1875(5) 0.6871(4) 0.5761(2) 0.0239(11) Uani 1 1 d . . . . .
C6 C 0.2353(5) 0.7877(4) 0.56496(19) 0.0225(10) Uani 1 1 d . . . . .
C7 C 0.1804(5) 0.8464(4) 0.5306(2) 0.0249(11) Uani 1 1 d . . . . .
H7A H 0.1045 0.8250 0.5138 0.030 Uiso 1 1 calc R . . . .
C8 C 0.2394(5) 0.9385(4) 0.5210(2) 0.0243(11) Uani 1 1 d . . . . .
C9 C 0.3531(5) 0.9676(4) 0.5488(2) 0.0232(10) Uani 1 1 d . . . . .
H9 H 0.3957 1.0276 0.5435 0.028 Uiso 1 1 calc R . . . .
C10 C 0.4006(5) 0.9070(4) 0.5835(2) 0.0233(10) Uani 1 1 d . . . . .
C11 C 0.5162(5) 0.9280(4) 0.6156(2) 0.0252(11) Uani 1 1 d . . . . .
C12 C 0.5848(5) 1.0180(4) 0.6182(2) 0.0283(12) Uani 1 1 d . . . . .
H12 H 0.5628 1.0676 0.5974 0.034 Uiso 1 1 calc R . . . .
C13 C 0.6871(6) 1.0344(4) 0.6522(2) 0.0337(13) Uani 1 1 d . . . . .
H13 H 0.7345 1.0947 0.6542 0.040 Uiso 1 1 calc R . . . .
C14 C 0.7173(6) 0.9601(5) 0.6827(2) 0.0335(13) Uani 1 1 d . . . . .
H14 H 0.7837 0.9698 0.7065 0.040 Uiso 1 1 calc R . . . .
C15 C 0.6452(5) 0.8692(4) 0.6772(2) 0.0300(12) Uani 1 1 d . . . . .
H15 H 0.6660 0.8184 0.6974 0.036 Uiso 1 1 calc R . . . .
C16 C 0.1862(5) 1.0003(4) 0.4830(2) 0.0239(11) Uani 1 1 d . . . . .
C17 C 0.2216(5) 1.1023(4) 0.4811(2) 0.0279(11) Uani 1 1 d . . . . .
H17 H 0.2767 1.1333 0.5058 0.033 Uiso 1 1 calc R . . . .
C18 C 0.1767(5) 1.1590(4) 0.4432(2) 0.0276(11) Uani 1 1 d . . . . .
H18 H 0.2023 1.2264 0.4426 0.033 Uiso 1 1 calc R . . . .
C19 C 0.0937(5) 1.1138(4) 0.4065(2) 0.0274(11) Uani 1 1 d . . . . .
C20 C 0.0553(5) 1.0125(4) 0.4090(2) 0.0281(11) Uani 1 1 d . . . . .
H20 H -0.0018 0.9819 0.3849 0.034 Uiso 1 1 calc R . . . .
C21 C 0.1002(5) 0.9581(4) 0.4463(2) 0.0284(11) Uani 1 1 d . . . . .
H21 H 0.0725 0.8912 0.4471 0.034 Uiso 1 1 calc R . . . .
C22 C 0.0914(5) 1.2495(4) 0.3489(2) 0.0294(12) Uani 1 1 d . . . . .
C23 C 0.0335(7) 1.2729(5) 0.2993(3) 0.0451(16) Uani 1 1 d . . . . .
H23A H 0.0092 1.2098 0.2799 0.054 Uiso 0.674(7) 1 calc R . P B 1
H23B H -0.0435 1.3119 0.3051 0.054 Uiso 0.674(7) 1 calc R . P B 1
H23C H 0.0919 1.2481 0.2738 0.054 Uiso 0.326(7) 1 calc R . P B 2
H23D H -0.0448 1.2328 0.2938 0.054 Uiso 0.326(7) 1 calc R . P B 2
C24 C 0.1217(10) 1.3298(9) 0.2709(4) 0.051(3) Uani 0.674(7) 1 d . . P B 1
H24A H 0.1951 1.2876 0.2632 0.061 Uiso 0.674(7) 1 calc R . P B 1
H24B H 0.1524 1.3888 0.2921 0.061 Uiso 0.674(7) 1 calc R . P B 1
C25 C 0.005(2) 1.3694(19) 0.2912(9) 0.051(3) Uani 0.326(7) 1 d . . P B 2
H25A H 0.0671 1.4136 0.3102 0.061 Uiso 0.326(7) 1 calc R . P B 2
H25B H -0.0778 1.3839 0.3054 0.061 Uiso 0.326(7) 1 calc R . P B 2
C26 C 0.001(3) 1.399(2) 0.2391(8) 0.041(5) Uani 0.326(7) 1 d . U P B 2
C27 C 0.0702(12) 1.3655(13) 0.2227(5) 0.049(3) Uani 0.674(7) 1 d . . P B 1
C28 C -0.0246(9) 1.4565(8) 0.2301(4) 0.034(2) Uani 0.674(7) 1 d . . P B 1
C29 C -0.0815(19) 1.4944(17) 0.2359(8) 0.034(2) Uani 0.326(7) 1 d . . P B 2
C30 C -0.0549(10) 1.5196(7) 0.1827(3) 0.063(2) Uani 1 1 d . . . . .
C31 C -0.1770(11) 1.5853(8) 0.1800(3) 0.075(3) Uani 1 1 d . . . . .
C32 C -0.1695(9) 1.6652(6) 0.1412(3) 0.059(2) Uani 1 1 d . . . . .
C33 C -0.3038(10) 1.7021(7) 0.1240(4) 0.073(3) Uani 1 1 d . . . . .
C34 C -0.2949(9) 1.8047(6) 0.0988(5) 0.074(3) Uani 1 1 d . . . . .
C35 C -0.4124(10) 1.8262(7) 0.0667(6) 0.094(4) Uani 1 1 d . . . . .
C36 C 0.5381(5) 0.6760(4) 0.5263(2) 0.0274(11) Uani 1 1 d . . . . .
H36 H 0.4912 0.7314 0.5180 0.033 Uiso 1 1 calc R . . . .
C37 C 0.6086(6) 0.6239(4) 0.4895(2) 0.0302(12) Uani 1 1 d . . . . .
H37 H 0.6102 0.6439 0.4574 0.036 Uiso 1 1 calc R . . . .
C38 C 0.6765(6) 0.5408(4) 0.5026(2) 0.0316(12) Uani 1 1 d . . . . .
H38 H 0.7242 0.5036 0.4789 0.038 Uiso 1 1 calc R . . . .
C39 C 0.6739(5) 0.5131(4) 0.5504(2) 0.0264(11) Uani 1 1 d . . . . .
H39 H 0.7196 0.4575 0.5593 0.032 Uiso 1 1 calc R . . . .
C40 C 0.6017(5) 0.5697(4) 0.5850(2) 0.0245(11) Uani 1 1 d . . . . .
C41 C 0.5922(5) 0.5474(4) 0.6372(2) 0.0264(11) Uani 1 1 d . . . . .
C42 C 0.6484(5) 0.4654(4) 0.6577(2) 0.0265(11) Uani 1 1 d . . . . .
H42 H 0.6973 0.4203 0.6379 0.032 Uiso 1 1 calc R . . . .
C43 C 0.6322(5) 0.4502(4) 0.7072(2) 0.0254(11) Uani 1 1 d . . . . .
C44 C 0.5579(5) 0.5205(4) 0.7355(2) 0.0289(12) Uani 1 1 d . . . . .
H44 H 0.5449 0.5135 0.7690 0.035 Uiso 1 1 calc R . . . .
C45 C 0.5033(5) 0.6020(4) 0.7127(2) 0.0261(11) Uani 1 1 d . . . . .
C46 C 0.4223(5) 0.6804(4) 0.7382(2) 0.0300(12) Uani 1 1 d . . . . .
C47 C 0.3957(6) 0.6859(5) 0.7878(2) 0.0408(15) Uani 1 1 d . . . . .
H47 H 0.4316 0.6402 0.8082 0.049 Uiso 1 1 calc R . . . .
C48 C 0.3147(7) 0.7604(6) 0.8072(3) 0.0492(18) Uani 1 1 d . . . . .
H48 H 0.2928 0.7640 0.8406 0.059 Uiso 1 1 calc R . . . .
C49 C 0.2665(7) 0.8301(5) 0.7761(3) 0.0441(16) Uani 1 1 d . . . . .
H49 H 0.2141 0.8822 0.7885 0.053 Uiso 1 1 calc R . . . .
C50 C 0.2973(6) 0.8207(4) 0.7269(2) 0.0318(12) Uani 1 1 d . . . . .
H50 H 0.2649 0.8672 0.7062 0.038 Uiso 1 1 calc R . . . .
C51 C 0.6901(6) 0.3638(4) 0.7298(2) 0.0318(12) Uani 1 1 d . . . . .
C52 C 0.7904(5) 0.3108(4) 0.7065(2) 0.0291(12) Uani 1 1 d . . . . .
H52 H 0.8187 0.3291 0.6761 0.035 Uiso 1 1 calc R . . . .
C53 C 0.8481(6) 0.2311(4) 0.7282(2) 0.0306(12) Uani 1 1 d . . . . .
H53 H 0.9132 0.1958 0.7117 0.037 Uiso 1 1 calc R . . . .
C54 C 0.8103(6) 0.2032(4) 0.7742(2) 0.0310(12) Uani 1 1 d . . . . .
C55 C 0.7094(6) 0.2551(5) 0.7973(2) 0.0377(14) Uani 1 1 d . . . . .
H55 H 0.6814 0.2369 0.8277 0.045 Uiso 1 1 calc R . . . .
C56 C 0.6505(6) 0.3333(5) 0.7754(2) 0.0381(14) Uani 1 1 d . . . . .
H56 H 0.5830 0.3665 0.7914 0.046 Uiso 1 1 calc R . . . .
C57 C 0.8652(6) 0.0882(5) 0.8387(2) 0.0367(14) Uani 1 1 d . . . . .
C58 C 0.9687(7) 0.0127(6) 0.8494(3) 0.0492(18) Uani 1 1 d . . . . .
H58A H 0.9727 -0.0382 0.8212 0.059 Uiso 1 1 calc R . . . .
H58B H 1.0508 0.0481 0.8529 0.059 Uiso 1 1 calc R . . . .
C59 C 0.9469(9) -0.0381(7) 0.8947(3) 0.067(3) Uani 1 1 d . . . . .
H59A H 0.9280 0.0130 0.9216 0.080 Uiso 1 1 calc R . . . .
H59B H 0.8720 -0.0822 0.8889 0.080 Uiso 1 1 calc R . . . .
C60 C 1.0537(7) -0.0981(6) 0.9107(3) 0.0488(18) Uani 1 1 d . . . . .
C61 C 1.0429(9) -0.1652(8) 0.9515(3) 0.071(3) Uani 1 1 d . . . . .
C62 C 1.1369(8) -0.2446(6) 0.9607(3) 0.0481(18) Uani 1 1 d . . . . .
C63 C 1.1465(11) -0.2958(8) 1.0066(3) 0.081(4) Uani 1 1 d . . . . .
C64 C 1.2115(8) -0.3943(5) 1.0086(3) 0.0477(17) Uani 1 1 d . . . . .
C65 C 1.2582(13) -0.4343(9) 1.0533(3) 0.092(4) Uani 1 1 d . . . . .
C66 C 1.2887(10) -0.5418(8) 1.0576(5) 0.073(3) Uani 1 1 d . . . . .
C67 C 1.386(2) -0.5716(17) 1.0941(8) 0.044(4) Uani 0.5 1 d . U P I 2
C68 C 1.327(3) -0.600(2) 1.0961(10) 0.079(7) Uani 0.5 1 d . . P I 1
C69 C 0.5352(11) 1.0150(9) 0.7929(4) 0.088(3) Uani 1 1 d . . . . .
H69A H 0.5917 1.0670 0.8085 0.132 Uiso 1 1 calc GR . . . .
H69B H 0.4514 1.0230 0.8063 0.132 Uiso 1 1 calc GR . . . .
H69C H 0.5305 1.0202 0.7576 0.132 Uiso 1 1 calc GR . . . .
C70 C 0.5826(16) 0.9085(9) 0.8736(5) 0.127(6) Uani 1 1 d . . . . .
H70A H 0.6197 0.8509 0.8873 0.190 Uiso 1 1 calc GR . . . .
H70B H 0.4942 0.9131 0.8822 0.190 Uiso 1 1 calc GR . . . .
H70C H 0.6277 0.9692 0.8868 0.190 Uiso 1 1 calc GR . . . .
C71 C 0.3734(7) 0.1910(6) 0.7000(3) 0.0512(17) Uani 1 1 d . . . . .
H71A H 0.3392 0.1280 0.7092 0.077 Uiso 0.5 1 calc R . P A 1
H71B H 0.4651 0.1905 0.7027 0.077 Uiso 0.5 1 calc R . P A 1
H71C H 0.3420 0.2460 0.7219 0.077 Uiso 0.5 1 calc R . P A 1
H71D H 0.3147 0.1678 0.7235 0.077 Uiso 0.5 1 calc R . P A 2
H71E H 0.4003 0.1344 0.6781 0.077 Uiso 0.5 1 calc R . P A 2
H71F H 0.4466 0.2227 0.7177 0.077 Uiso 0.5 1 calc R . P A 2
C72 C 0.1643(14) 0.2332(12) 0.6517(7) 0.048(3) Uani 0.5 1 d . . P A 1
H72A H 0.1599 0.2853 0.6788 0.072 Uiso 0.5 1 calc GR . P A 1
H72B H 0.1217 0.1729 0.6604 0.072 Uiso 0.5 1 calc GR . P A 1
H72C H 0.1233 0.2558 0.6225 0.072 Uiso 0.5 1 calc GR . P A 1
C73 C 0.1912(17) 0.1965(12) 0.6267(6) 0.049(4) Uani 0.5 1 d . . P A 2
H73A H 0.1431 0.2325 0.6033 0.074 Uiso 0.5 1 calc GR . P A 2
H73B H 0.1335 0.1648 0.6478 0.074 Uiso 0.5 1 calc GR . P A 2
H73C H 0.2413 0.1456 0.6089 0.074 Uiso 0.5 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.106(5) . ?
Ni1 N2 2.002(4) . ?
Ni1 N3 2.108(5) . ?
Ni1 N4 2.126(5) . ?
Ni1 N5 1.998(4) . ?
Ni1 N6 2.119(5) . ?
S1 O3 1.457(6) . ?
S1 C71 1.827(8) . ?
S1 C73 1.774(15) . ?
S2 O3 1.606(6) . ?
S2 C71 1.724(8) . ?
S2 C72 1.767(16) . ?
S3 O4 1.401(8) . ?
S3 C69 1.783(11) . ?
S3 C70 1.862(12) . ?
F1 C27 1.323(18) . ?
F2 C27 1.365(14) . ?
F3 C26 1.36(3) . ?
F4 C26 1.33(3) . ?
F5 C28 1.367(11) . ?
F6 C28 1.326(12) . ?
F7 C29 1.30(3) . ?
F8 C29 1.43(2) . ?
F9 C30 1.330(9) . ?
F10 C30 1.330(9) . ?
F11 C31 1.330(10) . ?
F12 C31 1.360(10) . ?
F13 C32 1.335(9) . ?
F14 C32 1.322(10) . ?
F15 C33 1.334(10) . ?
F16 C33 1.342(11) . ?
F17 C34 1.331(12) . ?
F18 C34 1.342(10) . ?
F19 C35 1.325(15) . ?
F20 C35 1.334(12) . ?
F21 C35 1.323(12) . ?
F22 C60 1.473(11) . ?
F23 C60 1.386(14) . ?
F24 C60 1.254(12) . ?
F25 C60 1.549(12) . ?
F26 C61 1.602(14) . ?
F27 C61 1.24(4) . ?
F28 C61 1.29(4) . ?
F29 C61 1.632(14) . ?
F30 C62 1.509(12) . ?
F31 C62 1.299(18) . ?
F32 C62 1.290(17) . ?
F33 C62 1.522(12) . ?
F34 C63 1.622(15) . ?
F35 C63 1.31(2) . ?
F36 C63 1.24(2) . ?
F37 C63 1.654(15) . ?
F38 C64 1.493(12) . ?
F39 C64 1.228(17) . ?
F40 C64 1.358(17) . ?
F41 C64 1.510(12) . ?
F42 C65 1.681(17) . ?
F43 C65 1.41(2) . ?
F44 C65 1.13(3) . ?
F45 C65 1.615(16) . ?
F46 C66 1.549(15) . ?
F47 C66 1.15(2) . ?
F48 C66 1.46(2) . ?
F49 C66 1.504(14) . ?
F50 C68 1.24(3) . ?
F51 C68 1.31(3) . ?
F52 C67 1.29(3) . ?
F53 C67 1.34(2) . ?
F54 C68 1.33(4) . ?
F55 C67 1.36(3) . ?
O1 C22 1.220(7) . ?
O2 C57 1.225(8) . ?
O5 H5A 0.8370 . ?
O5 H5B 0.8356 . ?
N1 C11 1.357(7) . ?
N1 C15 1.329(7) . ?
N2 C6 1.334(7) . ?
N2 C10 1.355(7) . ?
N3 C1 1.345(7) . ?
N3 C5 1.355(7) . ?
N4 C36 1.321(7) . ?
N4 C40 1.354(7) . ?
N5 C41 1.336(7) . ?
N5 C45 1.325(7) . ?
N6 C46 1.364(7) . ?
N6 C50 1.343(7) . ?
N7 H7 0.9927 . ?
N7 C19 1.401(7) . ?
N7 C22 1.376(7) . ?
N8 H8 0.9906 . ?
N8 C54 1.397(7) . ?
N8 C57 1.354(8) . ?
C1 H1 0.9300 . ?
C1 C2 1.379(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.371(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.386(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.395(8) . ?
C5 C6 1.476(7) . ?
C6 C7 1.382(8) . ?
C7 H7A 0.9300 . ?
C7 C8 1.407(8) . ?
C8 C9 1.416(8) . ?
C8 C16 1.473(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.376(7) . ?
C10 C11 1.475(7) . ?
C11 C12 1.377(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.390(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.375(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.404(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.402(8) . ?
C16 C21 1.390(8) . ?
C17 H17 0.9300 . ?
C17 C18 1.399(8) . ?
C18 H18 0.9300 . ?
C18 C19 1.384(8) . ?
C19 C20 1.402(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.368(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.514(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C23 H23D 0.9700 . ?
C23 C24 1.461(12) . ?
C23 C25 1.35(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C27 1.512(16) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.50(3) . ?
C26 C29 1.54(3) . ?
C27 C28 1.572(18) . ?
C28 C30 1.616(12) . ?
C29 C30 1.53(2) . ?
C30 C31 1.559(15) . ?
C31 C32 1.558(12) . ?
C32 C33 1.565(15) . ?
C33 C34 1.578(13) . ?
C34 C35 1.528(17) . ?
C36 H36 0.9300 . ?
C36 C37 1.387(8) . ?
C37 H37 0.9300 . ?
C37 C38 1.385(8) . ?
C38 H38 0.9300 . ?
C38 C39 1.372(8) . ?
C39 H39 0.9300 . ?
C39 C40 1.387(8) . ?
C40 C41 1.471(8) . ?
C41 C42 1.395(8) . ?
C42 H42 0.9300 . ?
C42 C43 1.381(8) . ?
C43 C44 1.404(8) . ?
C43 C51 1.476(7) . ?
C44 H44 0.9300 . ?
C44 C45 1.410(7) . ?
C45 C46 1.480(8) . ?
C46 C47 1.370(9) . ?
C47 H47 0.9300 . ?
C47 C48 1.384(9) . ?
C48 H48 0.9300 . ?
C48 C49 1.396(10) . ?
C49 H49 0.9300 . ?
C49 C50 1.368(9) . ?
C50 H50 0.9300 . ?
C51 C52 1.398(8) . ?
C51 C56 1.402(8) . ?
C52 H52 0.9300 . ?
C52 C53 1.393(8) . ?
C53 H53 0.9300 . ?
C53 C54 1.392(8) . ?
C54 C55 1.395(9) . ?
C55 H55 0.9300 . ?
C55 C56 1.383(8) . ?
C56 H56 0.9300 . ?
C57 C58 1.523(8) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C58 C59 1.469(9) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 C60 1.457(9) . ?
C60 C61 1.485(10) . ?
C61 C62 1.482(10) . ?
C62 C63 1.466(10) . ?
C63 C64 1.483(11) . ?
C64 C65 1.439(11) . ?
C65 C66 1.478(13) . ?
C66 C67 1.48(2) . ?
C66 C68 1.40(3) . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?
C71 H71D 0.9600 . ?
C71 H71E 0.9600 . ?
C71 H71F 0.9600 . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 154.67(17) . . ?
N1 Ni1 N4 96.15(18) . . ?
N1 Ni1 N6 89.07(18) . . ?
N2 Ni1 N1 77.64(18) . . ?
N2 Ni1 N3 77.70(17) . . ?
N2 Ni1 N4 95.34(17) . . ?
N2 Ni1 N6 109.14(17) . . ?
N3 Ni1 N4 91.81(18) . . ?
N3 Ni1 N6 93.58(18) . . ?
N5 Ni1 N1 106.29(18) . . ?
N5 Ni1 N2 172.53(18) . . ?
N5 Ni1 N3 98.87(17) . . ?
N5 Ni1 N4 78.04(18) . . ?
N5 Ni1 N6 77.54(18) . . ?
N6 Ni1 N4 155.52(17) . . ?
O3 S1 C71 105.7(4) . . ?
O3 S1 C73 104.8(7) . . ?
C73 S1 C71 97.8(6) . . ?
O3 S2 C71 104.2(4) . . ?
O3 S2 C72 105.0(6) . . ?
C71 S2 C72 96.7(7) . . ?
O4 S3 C69 109.7(5) . . ?
O4 S3 C70 100.6(7) . . ?
C69 S3 C70 97.4(6) . . ?
H5A O5 H5B 114.7 . . ?
C11 N1 Ni1 114.4(4) . . ?
C15 N1 Ni1 127.0(4) . . ?
C15 N1 C11 118.5(5) . . ?
C6 N2 Ni1 119.2(3) . . ?
C6 N2 C10 120.6(5) . . ?
C10 N2 Ni1 118.8(4) . . ?
C1 N3 Ni1 127.3(4) . . ?
C1 N3 C5 118.7(5) . . ?
C5 N3 Ni1 114.0(3) . . ?
C36 N4 Ni1 127.6(4) . . ?
C36 N4 C40 119.0(5) . . ?
C40 N4 Ni1 113.4(4) . . ?
C41 N5 Ni1 118.9(4) . . ?
C45 N5 Ni1 119.7(4) . . ?
C45 N5 C41 121.2(5) . . ?
C46 N6 Ni1 114.4(4) . . ?
C50 N6 Ni1 127.3(4) . . ?
C50 N6 C46 118.3(5) . . ?
C19 N7 H7 111.7 . . ?
C22 N7 H7 118.2 . . ?
C22 N7 C19 126.7(5) . . ?
C54 N8 H8 116.8 . . ?
C57 N8 H8 114.6 . . ?
C57 N8 C54 128.6(5) . . ?
N3 C1 H1 118.8 . . ?
N3 C1 C2 122.5(5) . . ?
C2 C1 H1 118.8 . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 119.1(5) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.5(5) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(5) . . ?
C5 C4 H4 120.5 . . ?
N3 C5 C4 121.2(5) . . ?
N3 C5 C6 115.0(5) . . ?
C4 C5 C6 123.8(5) . . ?
N2 C6 C5 113.4(5) . . ?
N2 C6 C7 121.3(5) . . ?
C7 C6 C5 125.3(5) . . ?
C6 C7 H7A 120.0 . . ?
C6 C7 C8 120.0(5) . . ?
C8 C7 H7A 120.0 . . ?
C7 C8 C9 117.0(5) . . ?
C7 C8 C16 121.2(5) . . ?
C9 C8 C16 121.8(5) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(5) . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C9 120.9(5) . . ?
N2 C10 C11 112.9(5) . . ?
C9 C10 C11 126.2(5) . . ?
N1 C11 C10 114.9(5) . . ?
N1 C11 C12 121.7(5) . . ?
C12 C11 C10 123.4(5) . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.6(5) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.1(5) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 120.9 . . ?
C13 C14 C15 118.2(5) . . ?
C15 C14 H14 120.9 . . ?
N1 C15 C14 122.8(5) . . ?
N1 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C17 C16 C8 122.2(5) . . ?
C21 C16 C8 120.7(5) . . ?
C21 C16 C17 117.1(5) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 C16 122.0(5) . . ?
C18 C17 H17 119.0 . . ?
C17 C18 H18 120.3 . . ?
C19 C18 C17 119.5(5) . . ?
C19 C18 H18 120.3 . . ?
N7 C19 C20 116.1(5) . . ?
C18 C19 N7 125.1(5) . . ?
C18 C19 C20 118.7(5) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.2(5) . . ?
C21 C20 H20 119.4 . . ?
C16 C21 H21 119.2 . . ?
C20 C21 C16 121.6(5) . . ?
C20 C21 H21 119.2 . . ?
O1 C22 N7 124.8(5) . . ?
O1 C22 C23 121.1(5) . . ?
N7 C22 C23 114.1(5) . . ?
C22 C23 H23A 109.1 . . ?
C22 C23 H23B 109.1 . . ?
C22 C23 H23C 107.2 . . ?
C22 C23 H23D 107.2 . . ?
H23A C23 H23B 107.9 . . ?
H23C C23 H23D 106.9 . . ?
C24 C23 C22 112.4(7) . . ?
C24 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
C25 C23 C22 120.3(13) . . ?
C25 C23 H23C 107.2 . . ?
C25 C23 H23D 107.2 . . ?
C23 C24 H24A 108.0 . . ?
C23 C24 H24B 108.0 . . ?
C23 C24 C27 117.0(9) . . ?
H24A C24 H24B 107.3 . . ?
C27 C24 H24A 108.0 . . ?
C27 C24 H24B 108.0 . . ?
C23 C25 H25A 107.4 . . ?
C23 C25 H25B 107.4 . . ?
C23 C25 C26 120(2) . . ?
H25A C25 H25B 107.0 . . ?
C26 C25 H25A 107.4 . . ?
C26 C25 H25B 107.4 . . ?
F3 C26 C25 110(2) . . ?
F3 C26 C29 106(2) . . ?
F4 C26 F3 110(2) . . ?
F4 C26 C25 114(2) . . ?
F4 C26 C29 106.4(18) . . ?
C25 C26 C29 110(2) . . ?
F1 C27 F2 108.6(12) . . ?
F1 C27 C24 111.8(12) . . ?
F1 C27 C28 108.9(9) . . ?
F2 C27 C24 108.2(10) . . ?
F2 C27 C28 105.1(12) . . ?
C24 C27 C28 114.0(11) . . ?
F5 C28 C27 108.2(9) . . ?
F5 C28 C30 104.2(7) . . ?
F6 C28 F5 107.5(8) . . ?
F6 C28 C27 111.7(9) . . ?
F6 C28 C30 106.8(8) . . ?
C27 C28 C30 117.6(9) . . ?
F7 C29 F8 106.2(18) . . ?
F7 C29 C26 112.8(17) . . ?
F7 C29 C30 111.9(15) . . ?
F8 C29 C26 108.7(16) . . ?
F8 C29 C30 116.6(14) . . ?
C30 C29 C26 100.7(16) . . ?
F9 C30 C28 105.5(7) . . ?
F9 C30 C29 123.3(10) . . ?
F9 C30 C31 106.8(7) . . ?
F10 C30 F9 110.5(7) . . ?
F10 C30 C28 106.1(7) . . ?
F10 C30 C29 113.9(9) . . ?
F10 C30 C31 106.4(7) . . ?
C29 C30 C31 92.7(10) . . ?
C31 C30 C28 121.3(8) . . ?
F11 C31 F12 108.0(7) . . ?
F11 C31 C30 111.1(9) . . ?
F11 C31 C32 107.6(8) . . ?
F12 C31 C30 108.0(8) . . ?
F12 C31 C32 108.4(8) . . ?
C32 C31 C30 113.6(7) . . ?
F13 C32 C31 108.9(7) . . ?
F13 C32 C33 106.3(7) . . ?
F14 C32 F13 110.1(7) . . ?
F14 C32 C31 108.5(8) . . ?
F14 C32 C33 109.6(7) . . ?
C31 C32 C33 113.4(8) . . ?
F15 C33 F16 109.8(7) . . ?
F15 C33 C32 107.9(9) . . ?
F15 C33 C34 108.7(8) . . ?
F16 C33 C32 110.0(7) . . ?
F16 C33 C34 108.0(9) . . ?
C32 C33 C34 112.4(7) . . ?
F17 C34 F18 110.2(8) . . ?
F17 C34 C33 108.1(9) . . ?
F17 C34 C35 108.0(8) . . ?
F18 C34 C33 109.3(7) . . ?
F18 C34 C35 106.9(10) . . ?
C35 C34 C33 114.3(8) . . ?
F19 C35 F20 107.2(12) . . ?
F19 C35 C34 113.0(8) . . ?
F20 C35 C34 109.1(10) . . ?
F21 C35 F19 108.6(10) . . ?
F21 C35 F20 108.0(8) . . ?
F21 C35 C34 110.8(12) . . ?
N4 C36 H36 118.4 . . ?
N4 C36 C37 123.2(5) . . ?
C37 C36 H36 118.4 . . ?
C36 C37 H37 121.3 . . ?
C38 C37 C36 117.3(5) . . ?
C38 C37 H37 121.3 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.4(5) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 120.7 . . ?
C38 C39 C40 118.6(5) . . ?
C40 C39 H39 120.7 . . ?
N4 C40 C39 121.4(5) . . ?
N4 C40 C41 115.2(5) . . ?
C39 C40 C41 123.4(5) . . ?
N5 C41 C40 114.3(5) . . ?
N5 C41 C42 120.5(5) . . ?
C42 C41 C40 125.2(5) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 C41 120.7(5) . . ?
C43 C42 H42 119.6 . . ?
C42 C43 C44 117.4(5) . . ?
C42 C43 C51 121.8(5) . . ?
C44 C43 C51 120.8(5) . . ?
C43 C44 H44 120.3 . . ?
C43 C44 C45 119.4(5) . . ?
C45 C44 H44 120.3 . . ?
N5 C45 C44 120.8(5) . . ?
N5 C45 C46 114.5(5) . . ?
C44 C45 C46 124.8(5) . . ?
N6 C46 C45 113.7(5) . . ?
N6 C46 C47 122.2(5) . . ?
C47 C46 C45 124.0(5) . . ?
C46 C47 H47 120.5 . . ?
C46 C47 C48 119.0(6) . . ?
C48 C47 H47 120.5 . . ?
C47 C48 H48 120.5 . . ?
C47 C48 C49 119.0(6) . . ?
C49 C48 H48 120.5 . . ?
C48 C49 H49 120.5 . . ?
C50 C49 C48 119.0(6) . . ?
C50 C49 H49 120.5 . . ?
N6 C50 C49 122.5(6) . . ?
N6 C50 H50 118.8 . . ?
C49 C50 H50 118.8 . . ?
C52 C51 C43 120.3(5) . . ?
C52 C51 C56 117.5(5) . . ?
C56 C51 C43 122.1(5) . . ?
C51 C52 H52 119.6 . . ?
C53 C52 C51 120.7(5) . . ?
C53 C52 H52 119.6 . . ?
C52 C53 H53 119.4 . . ?
C54 C53 C52 121.2(5) . . ?
C54 C53 H53 119.4 . . ?
C53 C54 N8 117.0(5) . . ?
C53 C54 C55 118.1(5) . . ?
C55 C54 N8 124.8(5) . . ?
C54 C55 H55 119.6 . . ?
C56 C55 C54 120.7(6) . . ?
C56 C55 H55 119.6 . . ?
C51 C56 H56 119.2 . . ?
C55 C56 C51 121.6(6) . . ?
C55 C56 H56 119.2 . . ?
O2 C57 N8 123.9(6) . . ?
O2 C57 C58 123.3(6) . . ?
N8 C57 C58 112.8(5) . . ?
C57 C58 H58A 108.9 . . ?
C57 C58 H58B 108.9 . . ?
H58A C58 H58B 107.7 . . ?
C59 C58 C57 113.3(6) . . ?
C59 C58 H58A 108.9 . . ?
C59 C58 H58B 108.9 . . ?
C58 C59 H59A 108.6 . . ?
C58 C59 H59B 108.6 . . ?
H59A C59 H59B 107.5 . . ?
C60 C59 C58 114.8(7) . . ?
C60 C59 H59A 108.6 . . ?
C60 C59 H59B 108.6 . . ?
F22 C60 C61 91.4(7) . . ?
F23 C60 F25 95.1(9) . . ?
F23 C60 C59 119.5(8) . . ?
F23 C60 C61 117.5(8) . . ?
F24 C60 F22 106.9(8) . . ?
F24 C60 C59 119.0(8) . . ?
F24 C60 C61 112.8(7) . . ?
C59 C60 F22 96.4(7) . . ?
C59 C60 F25 92.8(7) . . ?
C59 C60 C61 122.2(7) . . ?
C61 C60 F25 90.9(7) . . ?
F27 C61 F29 95.4(19) . . ?
F27 C61 C60 112.5(16) . . ?
F27 C61 C62 124.0(17) . . ?
F28 C61 F26 95(2) . . ?
F28 C61 C60 122.3(18) . . ?
F28 C61 C62 113.0(16) . . ?
C60 C61 F26 96.7(7) . . ?
C60 C61 F29 87.5(7) . . ?
C62 C61 F26 89.8(7) . . ?
C62 C61 F29 91.7(7) . . ?
C62 C61 C60 123.3(7) . . ?
F31 C62 F33 102.3(9) . . ?
F31 C62 C61 114.0(9) . . ?
F31 C62 C63 120.1(10) . . ?
F32 C62 F30 101.9(9) . . ?
F32 C62 C61 118.8(9) . . ?
F32 C62 C63 114.2(9) . . ?
C61 C62 F30 94.2(7) . . ?
C61 C62 F33 88.9(7) . . ?
C63 C62 F30 89.7(8) . . ?
C63 C62 F33 90.5(7) . . ?
C63 C62 C61 124.6(6) . . ?
F35 C63 F37 94.7(12) . . ?
F35 C63 C62 112.5(10) . . ?
F35 C63 C64 124.6(11) . . ?
F36 C63 F34 97.1(11) . . ?
F36 C63 C62 124.8(12) . . ?
F36 C63 C64 111.4(10) . . ?
C62 C63 F34 94.6(7) . . ?
C62 C63 F37 88.5(8) . . ?
C62 C63 C64 122.2(7) . . ?
C64 C63 F34 90.3(8) . . ?
C64 C63 F37 94.7(7) . . ?
F39 C64 F41 107.8(10) . . ?
F39 C64 C63 113.5(9) . . ?
F39 C64 C65 118.9(10) . . ?
F40 C64 F38 98.6(9) . . ?
F40 C64 C63 118.3(9) . . ?
F40 C64 C65 115.2(9) . . ?
C63 C64 F38 94.6(7) . . ?
C63 C64 F41 88.4(7) . . ?
C65 C64 F38 88.6(8) . . ?
C65 C64 F41 90.3(8) . . ?
C65 C64 C63 125.2(7) . . ?
F43 C65 F45 92.2(13) . . ?
F43 C65 C64 113.6(10) . . ?
F43 C65 C66 120.3(11) . . ?
F44 C65 F42 100.7(15) . . ?
F44 C65 C64 127.2(14) . . ?
F44 C65 C66 107.6(14) . . ?
C64 C65 F42 90.8(8) . . ?
C64 C65 F45 92.0(8) . . ?
C64 C65 C66 124.9(10) . . ?
C66 C65 F42 84.1(9) . . ?
C66 C65 F45 96.6(8) . . ?
F47 C66 F49 110.8(11) . . ?
F47 C66 C65 112.7(12) . . ?
F47 C66 C67 116.9(15) . . ?
F48 C66 F46 88.9(12) . . ?
F48 C66 C65 118.8(12) . . ?
C65 C66 F46 94.5(8) . . ?
C65 C66 F49 90.4(9) . . ?
C65 C66 C67 121.6(13) . . ?
C67 C66 F49 98.9(11) . . ?
C68 C66 F46 104.0(15) . . ?
C68 C66 F48 101.4(17) . . ?
C68 C66 C65 135.9(17) . . ?
F52 C67 F53 109.0(17) . . ?
F52 C67 F55 105.0(17) . . ?
F52 C67 C66 115.4(19) . . ?
F53 C67 F55 103.7(19) . . ?
F53 C67 C66 105.4(15) . . ?
F55 C67 C66 117.5(16) . . ?
F50 C68 F51 112(3) . . ?
F50 C68 F54 109(3) . . ?
F50 C68 C66 107(2) . . ?
F51 C68 F54 99(2) . . ?
F51 C68 C66 123(2) . . ?
F54 C68 C66 106(3) . . ?
S3 C69 H69A 109.5 . . ?
S3 C69 H69B 109.5 . . ?
S3 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
S3 C70 H70A 109.5 . . ?
S3 C70 H70B 109.5 . . ?
S3 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
S1 C71 H71D 109.5 . . ?
S1 C71 H71E 109.5 . . ?
S1 C71 H71F 109.5 . . ?
S2 C71 H71A 109.5 . . ?
S2 C71 H71B 109.5 . . ?
S2 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
H71D C71 H71E 109.5 . . ?
H71D C71 H71F 109.5 . . ?
H71E C71 H71F 109.5 . . ?
S2 C72 H72A 109.5 . . ?
S2 C72 H72B 109.5 . . ?
S2 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
S1 C73 H73A 109.5 . . ?
S1 C73 H73B 109.5 . . ?
S1 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.365
_oxdiff_exptl_absorpt_empirical_full_min 0.669
####################################################################### 
# 
# 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_3_THF
_database_code_depnum_ccdc_archive 'CCDC 1533112'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT340_3.THF               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01035 Ang.  
RESPONSE: The data strategy was calculated and collected in triclinic
space group P-1, and later experiment is appended to reach completeness 99%
in non-centrosymmetric space group.
;
# end Validation Reply Form
_audit_creation_date             2017-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H15 F15 N4 O, C4 H8 O'
_chemical_formula_sum            'C33 H23 F15 N4 O2'
_chemical_formula_weight         792.55
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N3 F15 O1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P 21 c n'
_space_group_name_Hall           'P -2n 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y, -z'
'x, -y+1/2, z+1/2'

_cell_length_a                   5.7081(5)
_cell_length_b                   10.0000(7)
_cell_length_c                   56.029(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3198.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8131
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.2260
_cell_measurement_theta_min      4.4720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81665
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.022
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            44193
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.728
_diffrn_reflns_theta_max         66.728
_diffrn_reflns_theta_min         4.491
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.50   10.00    --  -41.65 -37.00 150.00   66
  2  ω   -114.00 -72.00   1.50   10.00    --  -41.65-143.00 -91.00   28
  3  ω   -117.00 -54.00   1.50   10.00    --  -41.65 -19.00-120.00   42
  4  ω    -50.00 -14.00   1.50   10.00    --  -41.65 -19.00-120.00   24
  5  ω    -92.00  46.00   1.50   10.00    --  -41.65   0.00 -60.00   92
  6  ω     23.00  86.00   1.50   10.00    --   41.65-125.00 -30.00   42
  7  ω      9.00 117.00   1.50   10.00    --   41.65  77.00 120.00   72
  8  ω     11.00  83.00   1.50   10.00    --   41.65  68.00 -43.54   48
  9  ω      2.00  81.50   1.50   10.00    --   41.65 -99.00 150.00   53
 10  ω      9.00  67.50   1.50   10.00    --   41.65  77.00  30.00   39
 11  ω      9.00  67.50   1.50   10.00    --   41.65  77.00-150.00   39
 12  ω     63.00 108.00   1.50   40.00    --  106.66 -94.00 -90.00   30
 13  ω     75.00 100.50   1.50   40.00    --  106.66  75.00-127.03   17
 14  ω     24.00 108.00   1.50   40.00    --  106.66 -94.00 150.00   56
 15  ω     34.00  61.00   1.50   40.00    --  106.66 -94.00 -90.00   18
 16  ω     80.00 140.00   1.50   40.00    --  106.66  61.00 -60.00   40
 17  ω    124.00 178.00   1.50   40.00    --  106.66  77.00 -34.80   36
 18  ω     75.00 102.00   1.50   40.00    --  106.66  72.00  -3.06   18
 19  ω     78.00 118.50   1.50   40.00    --  106.66  61.00 120.00   27
 20  ω     91.00 118.00   1.50   40.00    --  106.66-125.00  90.00   18
 21  ω     74.00 101.00   1.50   40.00    --  106.66  77.00-150.00   18
 22  ω     78.00 105.00   1.50   40.00    --  106.66  61.00  90.00   18
 23  ω     74.00 107.00   1.50   40.00    --  106.66  77.00-180.00   22
 24  ω     74.00  99.50   1.50   40.00    --  106.66  77.00  90.00   17
 25  ω    121.00 175.00   1.50   40.00    --  106.66  77.00  90.00   36
 26  ω     74.00 110.00   1.50   40.00    --  106.66  77.00   0.00   24
 27  ω    114.00 141.00   1.50   40.00    --  106.66  77.00   0.00   18
 28  ω     78.00 105.00   1.50   40.00    --  106.66  61.00-180.00   18
 29  ω     78.00 177.00   1.50   40.00    --  106.66  61.00 150.00   66
 30  ω     78.00 105.00   1.50   40.00    --  106.66  61.00-150.00   18
 31  ω     34.00  61.00   1.50   40.00    --  106.66-125.00  90.00   18
 32  ω     74.00 101.00   1.50   40.00    --  106.66  77.00 -34.80   18
 33  ω     74.00 129.50   1.50   40.00    --  106.66  77.00 -90.00   37
 34  ω     78.00 123.00   1.50   40.00    --  106.66  61.00  30.00   30
 35  ω     94.00 178.00   1.50   40.00    --  106.66 125.00   0.00   56
 36  ω     34.00 139.00   1.50   40.00    --  106.66 -77.00 -30.00   70
 37  ω     74.00 176.00   1.50   40.00    --  106.66  77.00  60.00   68
 38  ω     78.00 177.00   1.50   40.00    --  106.66  61.00-120.00   66
 39  ω     78.00 111.00   1.50   40.00    --  106.66  61.00  60.00   22
 40  ω     74.00 101.00   1.50   40.00    --  106.66  77.00 -60.00   18
 41  ω     74.00 101.00   1.50   40.00    --  106.66  77.00  30.00   18
 42  ω     78.00 105.00   1.50   40.00    --  106.66  61.00   0.00   18
 43  ω    110.00 176.00   1.50   40.00    --  106.66  61.00-150.00   44
 44  ω     74.00 143.00   1.50   40.00    --  106.66  77.00 120.00   46
 45  ω     76.00 101.50   1.50   40.00    --  106.66  70.00 154.78   17
 46  ω    152.00 177.50   1.50   40.00    --  106.66  61.00  90.00   17
 47  ω     76.00 101.50   1.50   40.00    --  106.66  68.00  62.35   17
 48  ω     77.00 102.50   1.50   40.00    --  106.66  66.00-102.16   17
 49  ω     75.00 112.50   1.50   40.00    --  106.66  74.00 -48.11   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1940384000
_diffrn_orient_matrix_UB_12      -0.0829171000
_diffrn_orient_matrix_UB_13      0.0120670000
_diffrn_orient_matrix_UB_21      0.1047273000
_diffrn_orient_matrix_UB_22      -0.0330875000
_diffrn_orient_matrix_UB_23      -0.0246461000
_diffrn_orient_matrix_UB_31      0.1556910000
_diffrn_orient_matrix_UB_32      0.1256274000
_diffrn_orient_matrix_UB_33      0.0015021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4925
_reflns_number_total             5656
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 
;
 Flack x determined using 1656 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5656
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0726
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0392P)²+7.8485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1468
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C3(H3), C4(H4A), C7(H7), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F -1.0284(8) -0.3353(5) -0.58257(7) 0.0349(10) Uani 1 1 d . . . . .
F2 F -1.0695(8) -0.5225(5) -0.56307(7) 0.0384(11) Uani 1 1 d . . . . .
F3 F -0.6434(8) -0.2743(5) -0.56012(7) 0.0382(11) Uani 1 1 d . . . . .
F4 F -0.6073(9) -0.4727(5) -0.54490(8) 0.0478(13) Uani 1 1 d . . . . .
F5 F -0.9632(10) -0.4448(5) -0.51685(7) 0.0479(13) Uani 1 1 d . . . . .
F6 F -1.0951(8) -0.2725(5) -0.53589(7) 0.0419(12) Uani 1 1 d . . . . .
F7 F -0.7561(9) -0.1208(4) -0.52216(7) 0.0386(11) Uani 1 1 d . . . . .
F8 F -0.5397(7) -0.2890(5) -0.51059(7) 0.0354(10) Uani 1 1 d . . . . .
F9 F -0.8172(9) -0.3446(5) -0.47494(7) 0.0401(11) Uani 1 1 d . . . . .
F10 F -1.0915(7) -0.2111(5) -0.48812(7) 0.0347(10) Uani 1 1 d . . . . .
F11 F -0.8148(9) 0.0014(5) -0.48151(8) 0.0426(12) Uani 1 1 d . . . . .
F12 F -0.5193(8) -0.1262(5) -0.47200(8) 0.0458(13) Uani 1 1 d . . . . .
F13 F -0.7487(12) -0.2119(5) -0.43327(8) 0.0618(17) Uani 1 1 d . . . . .
F14 F -0.7443(10) 0.0012(5) -0.43558(8) 0.0504(13) Uani 1 1 d . . . . .
F15 F -1.0598(9) -0.1057(6) -0.44358(8) 0.0520(14) Uani 1 1 d . . . . .
O1 O -0.7213(11) -0.6323(5) -0.58769(9) 0.0362(13) Uani 1 1 d . . . . .
O2 O -0.7864(11) -0.1626(5) -0.61934(9) 0.0358(13) Uani 1 1 d . . . . .
N1 N 0.4295(12) -0.9072(6) -0.67955(11) 0.0362(15) Uani 1 1 d . . . . .
N2 N 0.4604(10) -0.5747(6) -0.70430(9) 0.0221(12) Uani 1 1 d . . . . .
N3 N 0.2691(11) -0.2484(7) -0.72287(10) 0.0310(14) Uani 1 1 d . . . . .
N4 N -0.6597(10) -0.4313(6) -0.60671(9) 0.0237(13) Uani 1 1 d . . . . .
H4 H -0.7113 -0.3505 -0.6073 0.028 Uiso 1 1 calc R . . . .
C1 C 0.5509(15) -1.0213(8) -0.68041(15) 0.0385(19) Uani 1 1 d . . . . .
H1 H 0.4882 -1.0957 -0.6728 0.046 Uiso 1 1 calc R . . . .
C2 C 0.7638(15) -1.0361(8) -0.69194(13) 0.0367(19) Uani 1 1 d . . . . .
H2 H 0.8415 -1.1179 -0.6919 0.044 Uiso 1 1 calc R . . . .
C3 C 0.8577(14) -0.9272(8) -0.70341(13) 0.0354(18) Uani 1 1 d . . . . .
H3 H 1.0005 -0.9334 -0.7113 0.042 Uiso 1 1 calc R . . . .
C4 C 0.7338(14) -0.8070(7) -0.70289(12) 0.0276(15) Uani 1 1 d . . . . .
H4A H 0.7925 -0.7316 -0.7106 0.033 Uiso 1 1 calc R . . . .
C5 C 0.5216(13) -0.8014(7) -0.69078(11) 0.0240(15) Uani 1 1 d . . . . .
C6 C 0.3890(12) -0.6740(7) -0.68957(11) 0.0228(15) Uani 1 1 d . . . . .
C7 C 0.1980(12) -0.6594(7) -0.67389(11) 0.0239(15) Uani 1 1 d . . . . .
H7 H 0.1523 -0.7302 -0.6642 0.029 Uiso 1 1 calc R . . . .
C8 C 0.0779(11) -0.5382(7) -0.67301(10) 0.0207(14) Uani 1 1 d . . . . .
C9 C 0.1483(12) -0.4384(7) -0.68829(10) 0.0230(15) Uani 1 1 d . . . . .
H9 H 0.0689 -0.3573 -0.6885 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3385(12) -0.4583(7) -0.70360(10) 0.0219(14) Uani 1 1 d . . . . .
C11 C 0.4200(12) -0.3501(7) -0.71945(11) 0.0224(14) Uani 1 1 d . . . . .
C12 C 0.6416(13) -0.3525(8) -0.72972(11) 0.0248(15) Uani 1 1 d . . . . .
H12 H 0.7435 -0.4232 -0.7267 0.030 Uiso 1 1 calc R . . . .
C13 C 0.7089(13) -0.2468(8) -0.74464(11) 0.0283(16) Uani 1 1 d . . . . .
H13 H 0.8556 -0.2461 -0.7518 0.034 Uiso 1 1 calc R . . . .
C14 C 0.5529(14) -0.1439(8) -0.74840(12) 0.0318(17) Uani 1 1 d . . . . .
H14 H 0.5909 -0.0727 -0.7583 0.038 Uiso 1 1 calc R . . . .
C15 C 0.3396(14) -0.1492(9) -0.73705(13) 0.0356(19) Uani 1 1 d . . . . .
H15 H 0.2368 -0.0783 -0.7395 0.043 Uiso 1 1 calc R . . . .
C16 C -0.1204(12) -0.5166(7) -0.65605(11) 0.0222(14) Uani 1 1 d . . . . .
C17 C -0.1472(13) -0.5946(7) -0.63566(11) 0.0264(16) Uani 1 1 d . . . . .
H17 H -0.0420 -0.6638 -0.6329 0.032 Uiso 1 1 calc R . . . .
C18 C -0.3261(14) -0.5724(8) -0.61930(12) 0.0295(17) Uani 1 1 d . . . . .
H18 H -0.3419 -0.6269 -0.6060 0.035 Uiso 1 1 calc R . . . .
C19 C -0.4801(12) -0.4680(7) -0.62318(11) 0.0215(14) Uani 1 1 d . . . . .
C20 C -0.4586(13) -0.3892(7) -0.64360(11) 0.0229(14) Uani 1 1 d . . . . .
H20 H -0.5648 -0.3204 -0.6464 0.028 Uiso 1 1 calc R . . . .
C21 C -0.2800(12) -0.4132(7) -0.65961(11) 0.0218(14) Uani 1 1 d . . . . .
H21 H -0.2659 -0.3592 -0.6730 0.026 Uiso 1 1 calc R . . . .
C22 C -0.7544(13) -0.5130(7) -0.59028(12) 0.0265(15) Uani 1 1 d . . . . .
C23 C -0.9095(13) -0.4363(8) -0.57197(12) 0.0276(16) Uani 1 1 d . . . . .
C24 C -0.7625(12) -0.3802(7) -0.55128(11) 0.0221(14) Uani 1 1 d . . . . .
C25 C -0.9004(12) -0.3359(8) -0.52916(12) 0.0283(17) Uani 1 1 d . . . . .
C26 C -0.7596(12) -0.2451(7) -0.51202(12) 0.0255(15) Uani 1 1 d . . . . .
C27 C -0.8572(12) -0.2278(8) -0.48674(12) 0.0258(16) Uani 1 1 d . . . . .
C28 C -0.7551(13) -0.1155(8) -0.47169(13) 0.0301(16) Uani 1 1 d . . . . .
C29 C -0.8338(14) -0.1097(9) -0.44547(13) 0.0336(18) Uani 1 1 d . . . . .
C30 C -0.7035(19) -0.0537(9) -0.60523(18) 0.054(3) Uani 1 1 d . . . . .
H30A H -0.5337 -0.0547 -0.6045 0.065 Uiso 1 1 calc R . . . .
H30B H -0.7647 -0.0598 -0.5891 0.065 Uiso 1 1 calc R . . . .
C31 C -0.7865(18) 0.0708(8) -0.61689(16) 0.046(2) Uani 1 1 d . . . . .
H31A H -0.6738 0.1026 -0.6285 0.055 Uiso 1 1 calc R . . . .
H31B H -0.8143 0.1406 -0.6052 0.055 Uiso 1 1 calc R . . . .
C32 C -1.0120(17) 0.0288(9) -0.62881(16) 0.045(2) Uani 1 1 d . . . . .
H32A H -1.1463 0.0604 -0.6198 0.054 Uiso 1 1 calc R . . . .
H32B H -1.0208 0.0644 -0.6449 0.054 Uiso 1 1 calc R . . . .
C33 C -1.006(2) -0.1200(10) -0.6292(2) 0.069(3) Uani 1 1 d . . . . .
H33A H -1.1345 -0.1559 -0.6199 0.083 Uiso 1 1 calc R . . . .
H33B H -1.0210 -0.1520 -0.6455 0.083 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C23 1.354(8) . ?
F2 C23 1.351(9) . ?
F3 C24 1.352(8) . ?
F4 C24 1.330(8) . ?
F5 C25 1.337(9) . ?
F6 C25 1.334(9) . ?
F7 C26 1.367(8) . ?
F8 C26 1.332(8) . ?
F9 C27 1.362(9) . ?
F10 C27 1.350(8) . ?
F11 C28 1.337(9) . ?
F12 C28 1.350(9) . ?
F13 C29 1.322(9) . ?
F14 C29 1.341(10) . ?
F15 C29 1.295(10) . ?
O1 C22 1.216(9) . ?
O2 C30 1.427(10) . ?
O2 C33 1.435(11) . ?
N1 C1 1.337(10) . ?
N1 C5 1.338(9) . ?
N2 C6 1.354(9) . ?
N2 C10 1.356(9) . ?
N3 C11 1.346(9) . ?
N3 C15 1.333(10) . ?
N4 C19 1.427(8) . ?
N4 C22 1.345(9) . ?
C1 C2 1.384(12) . ?
C2 C3 1.373(12) . ?
C3 C4 1.395(10) . ?
C4 C5 1.390(11) . ?
C5 C6 1.483(10) . ?
C6 C7 1.408(10) . ?
C7 C8 1.393(10) . ?
C8 C9 1.375(10) . ?
C8 C16 1.494(9) . ?
C9 C10 1.398(9) . ?
C10 C11 1.476(9) . ?
C11 C12 1.390(10) . ?
C12 C13 1.402(10) . ?
C13 C14 1.377(11) . ?
C14 C15 1.374(11) . ?
C16 C17 1.392(9) . ?
C16 C21 1.392(9) . ?
C17 C18 1.390(10) . ?
C18 C19 1.382(10) . ?
C19 C20 1.395(9) . ?
C20 C21 1.379(9) . ?
C22 C23 1.557(10) . ?
C23 C24 1.538(10) . ?
C24 C25 1.534(9) . ?
C25 C26 1.547(10) . ?
C26 C27 1.532(9) . ?
C27 C28 1.520(11) . ?
C28 C29 1.538(10) . ?
C30 C31 1.483(12) . ?
C31 C32 1.510(12) . ?
C32 C33 1.488(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C30 O2 C33 106.1(7) . . ?
C1 N1 C5 117.0(7) . . ?
C6 N2 C10 117.2(6) . . ?
C15 N3 C11 117.0(6) . . ?
C22 N4 C19 125.1(6) . . ?
N1 C1 C2 124.3(8) . . ?
C3 C2 C1 118.4(7) . . ?
C2 C3 C4 118.4(7) . . ?
C5 C4 C3 119.2(7) . . ?
N1 C5 C4 122.7(7) . . ?
N1 C5 C6 117.2(6) . . ?
C4 C5 C6 120.1(6) . . ?
N2 C6 C5 116.7(6) . . ?
N2 C6 C7 122.5(6) . . ?
C7 C6 C5 120.9(6) . . ?
C8 C7 C6 119.6(6) . . ?
C7 C8 C16 121.4(6) . . ?
C9 C8 C7 117.7(6) . . ?
C9 C8 C16 120.8(6) . . ?
C8 C9 C10 120.4(7) . . ?
N2 C10 C9 122.6(6) . . ?
N2 C10 C11 116.8(6) . . ?
C9 C10 C11 120.6(6) . . ?
N3 C11 C10 116.0(6) . . ?
N3 C11 C12 122.5(7) . . ?
C12 C11 C10 121.5(6) . . ?
C11 C12 C13 118.9(7) . . ?
C14 C13 C12 118.6(7) . . ?
C15 C14 C13 118.3(7) . . ?
N3 C15 C14 124.9(8) . . ?
C17 C16 C8 121.6(6) . . ?
C17 C16 C21 117.5(6) . . ?
C21 C16 C8 120.8(6) . . ?
C18 C17 C16 122.2(7) . . ?
C19 C18 C17 119.0(6) . . ?
C18 C19 N4 123.3(6) . . ?
C18 C19 C20 120.0(6) . . ?
C20 C19 N4 116.6(6) . . ?
C21 C20 C19 120.0(6) . . ?
C20 C21 C16 121.3(6) . . ?
O1 C22 N4 128.0(7) . . ?
O1 C22 C23 119.5(6) . . ?
N4 C22 C23 112.3(6) . . ?
F1 C23 C22 111.3(5) . . ?
F1 C23 C24 109.4(6) . . ?
F2 C23 F1 107.4(6) . . ?
F2 C23 C22 108.2(6) . . ?
F2 C23 C24 108.9(5) . . ?
C24 C23 C22 111.5(6) . . ?
F3 C24 C23 106.5(5) . . ?
F3 C24 C25 109.2(6) . . ?
F4 C24 F3 108.0(6) . . ?
F4 C24 C23 108.2(6) . . ?
F4 C24 C25 109.0(5) . . ?
C25 C24 C23 115.8(6) . . ?
F5 C25 C24 108.6(6) . . ?
F5 C25 C26 107.3(6) . . ?
F6 C25 F5 108.0(6) . . ?
F6 C25 C24 109.7(6) . . ?
F6 C25 C26 109.2(6) . . ?
C24 C25 C26 113.8(6) . . ?
F7 C26 C25 106.5(6) . . ?
F7 C26 C27 106.7(6) . . ?
F8 C26 F7 108.1(6) . . ?
F8 C26 C25 109.5(6) . . ?
F8 C26 C27 108.9(6) . . ?
C27 C26 C25 116.8(6) . . ?
F9 C27 C26 106.9(6) . . ?
F9 C27 C28 107.5(6) . . ?
F10 C27 F9 107.5(6) . . ?
F10 C27 C26 108.7(5) . . ?
F10 C27 C28 108.7(6) . . ?
C28 C27 C26 117.2(6) . . ?
F11 C28 F12 108.6(7) . . ?
F11 C28 C27 108.7(6) . . ?
F11 C28 C29 106.6(6) . . ?
F12 C28 C27 108.5(6) . . ?
F12 C28 C29 107.9(6) . . ?
C27 C28 C29 116.5(7) . . ?
F13 C29 F14 106.6(6) . . ?
F13 C29 C28 111.0(7) . . ?
F14 C29 C28 108.3(7) . . ?
F15 C29 F13 110.4(7) . . ?
F15 C29 F14 108.6(7) . . ?
F15 C29 C28 111.7(6) . . ?
O2 C30 C31 106.9(7) . . ?
C30 C31 C32 103.5(7) . . ?
C33 C32 C31 105.4(8) . . ?
O2 C33 C32 108.1(8) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.552
_oxdiff_exptl_absorpt_empirical_full_min 0.782
####################################################################### 
# 
# 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_3_CHCl3
_database_code_depnum_ccdc_archive 'CCDC 1533113'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
_audit_creation_date             2016-10-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C29 H15 F15 N4 O, C H Cl3'
_chemical_formula_sum            'C30 H16 Cl3 F15 N4 O'
_chemical_formula_weight         839.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H20 N4 O F20'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.62249(13)
_cell_length_b                   60.950(3)
_cell_length_c                   9.3539(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.250(3)
_cell_angle_gamma                90
_cell_volume                     3163.84(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    123.0(3)
_cell_measurement_theta_max      73.9290
_cell_measurement_theta_min      4.3280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82305
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.0833
_exptl_crystal_size_mid          0.0409
_exptl_crystal_size_min          0.039
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -72
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9579
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.746
_diffrn_reflns_theta_max         66.746
_diffrn_reflns_theta_min         4.352
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00  -11.20   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 126

#__ type_ start__ end____ width___ exp.time_
  2 omega -115.00  -13.90   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013  -57.0000  -30.0000 337

#__ type_ start__ end____ width___ exp.time_
  3 omega   -3.00   30.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000  120.0000 110

#__ type_ start__ end____ width___ exp.time_
  4 omega   35.00   96.20   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -45.0000  -60.0000 204

#__ type_ start__ end____ width___ exp.time_
  5 omega   22.00  157.00   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601    0.0000 -150.0000 450

#__ type_ start__ end____ width___ exp.time_
  6 omega   44.00   88.10   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -45.0000 -150.0000 147

#__ type_ start__ end____ width___ exp.time_
  7 omega   30.00   99.00   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000  -30.0000 230

#__ type_ start__ end____ width___ exp.time_
  8 omega   31.00   67.00   0.3000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000    0.0000 120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.2531690000
_diffrn_orient_matrix_UB_12      -0.0052497000
_diffrn_orient_matrix_UB_13      -0.0339747000
_diffrn_orient_matrix_UB_21      0.1119021000
_diffrn_orient_matrix_UB_22      0.0071203000
_diffrn_orient_matrix_UB_23      0.1542058000
_diffrn_orient_matrix_UB_31      -0.0224298000
_diffrn_orient_matrix_UB_32      -0.0236773000
_diffrn_orient_matrix_UB_33      0.0537749000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4423
_reflns_number_total             5545
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         5545
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0489
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0554P)²+1.7779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1262
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 F25-C34
 1.32 with sigma of 0.02
 F26-C35
 1.32 with sigma of 0.02
 C34-F23
 1.32 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.01
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C34) = Uanis(C35)
Uanis(C25) = Uanis(C24)
4. Others
 Sof(C25)=Sof(F3)=Sof(F5)=1-FVAR(1)
 Sof(C24)=Sof(F4)=Sof(F6)=FVAR(1)
 Sof(C27)=Sof(F8)=Sof(F10)=1-FVAR(2)
 Sof(C26)=Sof(F7)=Sof(F9)=FVAR(2)
 Sof(C29)=Sof(F13)=Sof(F14)=1-FVAR(3)
 Sof(C28)=Sof(F11)=Sof(F12)=FVAR(3)
 Sof(C32)=Sof(F19)=Sof(F20)=1-FVAR(4)
 Sof(C33)=Sof(F21)=Sof(F22)=FVAR(4)
 Sof(C35)=Sof(F25)=Sof(F27)=Sof(F28)=1-FVAR(5)
 Sof(C34)=Sof(F23)=Sof(F24)=Sof(F26)=FVAR(5)
 Sof(C30)=Sof(F17)=Sof(F18)=1-FVAR(6)
 Sof(C31)=Sof(F15)=Sof(F16)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C36(H36)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), N4(H4A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 2.2300(6) 0.17951(5) 0.1561(3) 0.0356(7) Uani 1 1 d . . . . .
H1 H 2.1754 0.1708 0.0759 0.043 Uiso 1 1 calc R . . . .
C2 C 2.4325(6) 0.19223(5) 0.1523(3) 0.0361(7) Uani 1 1 d . . . . .
H2 H 2.5128 0.1919 0.0728 0.043 Uiso 1 1 calc R . . . .
C3 C 2.5113(5) 0.20537(5) 0.2701(3) 0.0354(7) Uani 1 1 d . . . . .
H3 H 2.6461 0.2142 0.2713 0.042 Uiso 1 1 calc R . . . .
C4 C 2.3873(5) 0.20524(5) 0.3871(3) 0.0323(6) Uani 1 1 d . . . . .
H4 H 2.4367 0.2141 0.4671 0.039 Uiso 1 1 calc R . . . .
C5 C 2.1888(5) 0.19164(4) 0.3827(3) 0.0268(6) Uani 1 1 d . . . . .
C6 C 2.0583(5) 0.18994(4) 0.5087(3) 0.0254(5) Uani 1 1 d . . . . .
C7 C 1.8792(5) 0.17427(4) 0.5120(3) 0.0260(5) Uani 1 1 d . . . . .
H7 H 1.8426 0.1645 0.4354 0.031 Uiso 1 1 calc R . . . .
C8 C 1.7544(5) 0.17309(4) 0.6285(3) 0.0255(5) Uani 1 1 d . . . . .
C9 C 1.8225(5) 0.18808(4) 0.7413(3) 0.0252(5) Uani 1 1 d . . . . .
H9 H 1.7449 0.1881 0.8219 0.030 Uiso 1 1 calc R . . . .
C10 C 2.0071(5) 0.20300(4) 0.7318(3) 0.0241(5) Uani 1 1 d . . . . .
C11 C 2.0821(5) 0.21893(4) 0.8513(3) 0.0245(5) Uani 1 1 d . . . . .
C12 C 2.2946(5) 0.23104(4) 0.8576(3) 0.0279(6) Uani 1 1 d . . . . .
H12 H 2.3933 0.2292 0.7877 0.033 Uiso 1 1 calc R . . . .
C13 C 2.3558(5) 0.24585(5) 0.9695(3) 0.0318(6) Uani 1 1 d . . . . .
H13 H 2.4954 0.2542 0.9756 0.038 Uiso 1 1 calc R . . . .
C14 C 2.2058(5) 0.24801(4) 1.0720(3) 0.0316(6) Uani 1 1 d . . . . .
H14 H 2.2425 0.2578 1.1489 0.038 Uiso 1 1 calc R . . . .
C15 C 1.9990(5) 0.23524(5) 1.0573(3) 0.0315(6) Uani 1 1 d . . . . .
H15 H 1.8988 0.2368 1.1267 0.038 Uiso 1 1 calc R . . . .
C16 C 1.5576(5) 0.15691(4) 0.6327(3) 0.0252(5) Uani 1 1 d . . . . .
C17 C 1.4595(5) 0.15301(5) 0.7578(3) 0.0330(6) Uani 1 1 d . . . . .
H17 H 1.5215 0.1606 0.8420 0.040 Uiso 1 1 calc R . . . .
C18 C 1.2731(5) 0.13832(5) 0.7615(3) 0.0334(6) Uani 1 1 d . . . . .
H18 H 1.2099 0.1362 0.8465 0.040 Uiso 1 1 calc R . . . .
C19 C 1.1807(5) 0.12665(4) 0.6367(3) 0.0267(6) Uani 1 1 d . . . . .
C20 C 1.2769(5) 0.13018(5) 0.5112(3) 0.0301(6) Uani 1 1 d . . . . .
H20 H 1.2166 0.1224 0.4276 0.036 Uiso 1 1 calc R . . . .
C21 C 1.4610(5) 0.14504(5) 0.5090(3) 0.0295(6) Uani 1 1 d . . . . .
H21 H 1.5222 0.1472 0.4234 0.035 Uiso 1 1 calc R . . . .
C22 C 0.8749(5) 0.10504(5) 0.7383(3) 0.0326(6) Uani 1 1 d . . . . .
C23 C 0.7083(5) 0.08489(5) 0.7013(3) 0.0344(7) Uani 1 1 d . . . . .
C24 C 0.852(3) 0.06244(19) 0.7413(19) 0.0364(17) Uani 0.74(2) 1 d . . P A 1
C25 C 0.822(8) 0.0667(6) 0.735(6) 0.0364(17) Uani 0.26(2) 1 d . . P A 2
C26 C 0.687(2) 0.0431(2) 0.7372(17) 0.040(2) Uani 0.785(6) 1 d . . P A 2
C27 C 0.727(8) 0.0387(7) 0.724(6) 0.039(9) Uani 0.215(6) 1 d . U P A 1
C28 C 0.8199(10) 0.02096(9) 0.7248(9) 0.0453(14) Uani 0.773(6) 1 d . . P A 2
C29 C 0.816(4) 0.0197(3) 0.801(3) 0.046(5) Uani 0.227(6) 1 d . . P A 1
C30 C 0.6807(14) 0.00031(13) 0.7620(11) 0.049(2) Uani 0.772(6) 1 d . . P A 2
F17 F 0.4620(11) 0.00140(12) 0.6974(9) 0.068(2) Uani 0.772(6) 1 d . . P A 2
C32 C 0.786(3) -0.0224(3) 0.825(2) 0.052(4) Uani 0.250(6) 1 d . . P A 1
C33 C 0.7855(9) -0.02175(8) 0.7183(9) 0.0570(16) Uani 0.750(6) 1 d . . P A 2
C34 C 0.683(4) -0.0441(16) 0.738(5) 0.062(2) Uani 0.237(8) 1 d D . P A 1
C35 C 0.6709(16) -0.0427(4) 0.7701(13) 0.062(2) Uani 0.763(8) 1 d D . P A 2
F1 F 0.5262(3) 0.08619(3) 0.7790(2) 0.0435(5) Uani 1 1 d . . . . .
F2 F 0.6117(4) 0.08447(3) 0.5606(2) 0.0486(5) Uani 1 1 d . . . . .
F3 F 0.882(5) 0.0636(2) 0.9089(16) 0.060(5) Uani 0.26(2) 1 d . . P A 2
F4 F 0.9917(13) 0.06551(6) 0.8598(9) 0.058(2) Uani 0.74(2) 1 d . . P A 1
F5 F 1.061(3) 0.06204(18) 0.722(4) 0.062(7) Uani 0.26(2) 1 d . . P A 2
F6 F 0.9842(13) 0.06089(5) 0.6296(10) 0.0496(19) Uani 0.74(2) 1 d . . P A 1
F7 F 0.6020(6) 0.04290(4) 0.8652(4) 0.0640(11) Uani 0.785(6) 1 d . . P A 2
F8 F 0.4890(19) 0.04312(17) 0.7257(16) 0.046(3) Uani 0.215(6) 1 d . . P A 1
F9 F 0.4969(5) 0.04415(5) 0.6320(5) 0.0554(9) Uani 0.785(6) 1 d . . P A 2
F10 F 0.7430(19) 0.03745(14) 0.5759(10) 0.052(3) Uani 0.215(6) 1 d . . P A 1
F11 F 0.8557(6) 0.01918(4) 0.5869(4) 0.0617(10) Uani 0.773(6) 1 d . . P A 2
F12 F 1.030(2) 0.0215(2) 0.8117(12) 0.074(4) Uani 0.773(6) 1 d . . P A 2
F13 F 1.067(7) 0.0213(6) 0.815(3) 0.037(4) Uani 0.227(6) 1 d . . P A 1
F14 F 0.754(2) 0.02100(15) 0.9332(11) 0.061(3) Uani 0.227(6) 1 d . . P A 1
F18 F 0.6769(7) -0.00009(5) 0.9036(4) 0.0769(13) Uani 0.772(6) 1 d . . P A 2
C31 C 0.733(5) -0.0024(5) 0.730(3) 0.038(6) Uani 0.228(6) 1 d . U P A 1
F15 F 0.843(2) -0.00514(16) 0.6152(11) 0.065(4) Uani 0.228(6) 1 d . . P A 1
F16 F 0.461(5) 0.0001(5) 0.676(3) 0.063(8) Uani 0.228(6) 1 d . . P A 1
F19 F 0.650(2) -0.02089(16) 0.9353(11) 0.069(3) Uani 0.250(6) 1 d . . P A 1
F20 F 1.023(2) -0.02252(17) 0.8759(12) 0.050(3) Uani 0.250(6) 1 d . . P A 1
F21 F 1.0139(8) -0.02295(7) 0.7773(9) 0.106(2) Uani 0.750(6) 1 d . U P A 2
F22 F 0.7770(9) -0.02283(5) 0.5771(5) 0.0920(15) Uani 0.750(6) 1 d . U P A 2
F23 F 0.854(2) -0.0487(2) 0.6557(12) 0.067(4) Uani 0.237(8) 1 d D . P A 1
F24 F 0.753(2) -0.06014(15) 0.8517(13) 0.069(4) Uani 0.237(8) 1 d . . P A 1
F25 F 0.4408(13) -0.04292(12) 0.7120(10) 0.091(3) Uani 0.763(8) 1 d D . P A 1
F26 F 0.465(4) -0.0424(5) 0.683(2) 0.090(10) Uani 0.237(8) 1 d D . P A 2
F27 F 0.7508(7) -0.06008(5) 0.7112(6) 0.0908(18) Uani 0.763(8) 1 d . . P A 2
F28 F 0.6755(12) -0.04435(7) 0.9026(5) 0.126(2) Uani 0.763(8) 1 d . . P A 2
N1 N 1.9346(4) 0.22097(4) 0.9504(3) 0.0282(5) Uani 1 1 d . . . . .
N2 N 2.1240(4) 0.20420(3) 0.6178(3) 0.0255(5) Uani 1 1 d . . . . .
N3 N 2.1073(4) 0.17889(4) 0.2671(3) 0.0324(5) Uani 1 1 d . . . . .
N4 N 0.9956(4) 0.11079(4) 0.6308(3) 0.0300(5) Uani 1 1 d . . . . .
H4A H 0.9558 0.1041 0.5496 0.036 Uiso 1 1 calc R . . . .
O1 O 0.8906(4) 0.11329(4) 0.8565(3) 0.0442(6) Uani 1 1 d . . . . .
C36 C 0.6571(6) 0.11304(5) 1.1262(4) 0.0397(7) Uani 1 1 d . . . . .
H36 H 0.6752 0.1098 1.0259 0.048 Uiso 1 1 calc R . . . .
Cl1 Cl 0.79206(13) 0.13866(2) 1.17483(8) 0.03855(19) Uani 1 1 d . . . . .
Cl2 Cl 0.34854(14) 0.11380(2) 1.13772(10) 0.0569(3) Uani 1 1 d . . . . .
Cl3 Cl 0.80215(16) 0.09221(2) 1.23946(12) 0.0559(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9300 . ?
C1 C2 1.382(5) . ?
C1 N3 1.336(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.377(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.389(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.385(4) . ?
C5 C6 1.489(4) . ?
C5 N3 1.351(4) . ?
C6 C7 1.392(4) . ?
C6 N2 1.346(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.389(4) . ?
C8 C9 1.402(4) . ?
C8 C16 1.487(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.394(4) . ?
C10 C11 1.489(4) . ?
C10 N2 1.342(3) . ?
C11 C12 1.397(4) . ?
C11 N1 1.345(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.383(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.382(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.387(4) . ?
C15 H15 0.9300 . ?
C15 N1 1.331(4) . ?
C16 C17 1.392(4) . ?
C16 C21 1.398(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.383(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.395(4) . ?
C19 C20 1.386(4) . ?
C19 N4 1.415(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.378(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.550(4) . ?
C22 N4 1.347(4) . ?
C22 O1 1.205(4) . ?
C23 C24 1.603(10) . ?
C23 C25 1.29(3) . ?
C23 F1 1.350(3) . ?
C23 F2 1.341(4) . ?
C24 C27 1.60(5) . ?
C24 F4 1.265(18) . ?
C24 F6 1.378(16) . ?
C25 C26 1.63(5) . ?
C25 F3 1.62(6) . ?
C25 F5 1.40(4) . ?
C26 C28 1.556(11) . ?
C26 F7 1.357(14) . ?
C26 F9 1.332(15) . ?
C27 C29 1.41(5) . ?
C27 F8 1.37(4) . ?
C27 F10 1.40(5) . ?
C28 C30 1.551(9) . ?
C28 F11 1.342(8) . ?
C28 F12 1.322(15) . ?
C29 F13 1.40(4) . ?
C29 F14 1.34(2) . ?
C29 C31 1.54(4) . ?
C30 F17 1.282(12) . ?
C30 C33 1.549(9) . ?
C30 F18 1.328(10) . ?
C32 C34 1.61(8) . ?
C32 C31 1.50(3) . ?
C32 F19 1.38(2) . ?
C32 F20 1.343(19) . ?
C33 C35 1.54(3) . ?
C33 F21 1.316(8) . ?
C33 F22 1.316(9) . ?
C34 F23 1.36(2) . ?
C34 F24 1.45(9) . ?
C34 F25 1.35(2) . ?
C35 F26 1.301(17) . ?
C35 F27 1.309(19) . ?
C35 F28 1.240(15) . ?
C31 F15 1.33(3) . ?
C31 F16 1.54(4) . ?
N4 H4A 0.8600 . ?
C36 H36 0.9800 . ?
C36 Cl1 1.764(3) . ?
C36 Cl2 1.756(3) . ?
C36 Cl3 1.767(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 117.8 . . ?
N3 C1 H1 117.8 . . ?
N3 C1 C2 124.5(3) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 C1 117.8(3) . . ?
C3 C2 H2 121.1 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.3(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.5 . . ?
C5 C4 C3 118.9(3) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C6 121.0(3) . . ?
N3 C5 C4 122.4(3) . . ?
N3 C5 C6 116.5(2) . . ?
C7 C6 C5 121.1(2) . . ?
N2 C6 C5 116.4(2) . . ?
N2 C6 C7 122.5(2) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.7(3) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C9 116.5(2) . . ?
C7 C8 C16 121.8(2) . . ?
C9 C8 C16 121.8(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 C8 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C11 120.1(2) . . ?
N2 C10 C9 123.5(2) . . ?
N2 C10 C11 116.4(2) . . ?
C12 C11 C10 120.9(2) . . ?
N1 C11 C10 116.5(2) . . ?
N1 C11 C12 122.7(2) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.8(3) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 H14 120.9 . . ?
C13 C14 C15 118.2(3) . . ?
C15 C14 H14 120.9 . . ?
C14 C15 H15 117.8 . . ?
N1 C15 C14 124.3(3) . . ?
N1 C15 H15 117.8 . . ?
C17 C16 C8 122.2(2) . . ?
C17 C16 C21 117.0(2) . . ?
C21 C16 C8 120.9(2) . . ?
C16 C17 H17 118.8 . . ?
C18 C17 C16 122.4(3) . . ?
C18 C17 H17 118.8 . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.4(3) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 N4 123.6(2) . . ?
C20 C19 C18 119.1(3) . . ?
C20 C19 N4 117.2(2) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20 119.6 . . ?
C16 C21 H21 119.3 . . ?
C20 C21 C16 121.4(3) . . ?
C20 C21 H21 119.3 . . ?
N4 C22 C23 113.5(3) . . ?
O1 C22 C23 119.2(3) . . ?
O1 C22 N4 127.3(3) . . ?
C22 C23 C24 111.1(6) . . ?
C25 C23 C22 112(2) . . ?
C25 C23 F1 108(2) . . ?
C25 C23 F2 109(3) . . ?
F1 C23 C22 108.5(2) . . ?
F1 C23 C24 108.8(6) . . ?
F2 C23 C22 111.7(2) . . ?
F2 C23 C24 108.8(7) . . ?
F2 C23 F1 107.9(2) . . ?
C23 C24 C27 123.3(18) . . ?
F4 C24 C23 107.2(9) . . ?
F4 C24 C27 115(2) . . ?
F4 C24 F6 110.0(10) . . ?
F6 C24 C23 101.2(10) . . ?
F6 C24 C27 98.1(18) . . ?
C23 C25 C26 123(3) . . ?
C23 C25 F3 111(3) . . ?
C23 C25 F5 127(4) . . ?
F3 C25 C26 85(3) . . ?
F5 C25 C26 106(2) . . ?
F5 C25 F3 91(3) . . ?
C28 C26 C25 122.2(16) . . ?
F7 C26 C25 104(2) . . ?
F7 C26 C28 107.5(9) . . ?
F9 C26 C25 105.5(19) . . ?
F9 C26 C28 109.0(10) . . ?
F9 C26 F7 107.5(9) . . ?
C29 C27 C24 125(3) . . ?
F8 C27 C24 104(2) . . ?
F8 C27 C29 115(4) . . ?
F8 C27 F10 104(3) . . ?
F10 C27 C24 93(3) . . ?
F10 C27 C29 113(3) . . ?
C30 C28 C26 114.8(7) . . ?
F11 C28 C26 106.9(7) . . ?
F11 C28 C30 108.0(6) . . ?
F12 C28 C26 109.1(9) . . ?
F12 C28 C30 108.4(8) . . ?
F12 C28 F11 109.6(7) . . ?
C27 C29 C31 116(3) . . ?
F13 C29 C27 105(3) . . ?
F13 C29 C31 109(2) . . ?
F14 C29 C27 107(2) . . ?
F14 C29 F13 108(2) . . ?
F14 C29 C31 110.1(18) . . ?
F17 C30 C28 109.5(7) . . ?
F17 C30 C33 107.3(8) . . ?
F17 C30 F18 107.6(7) . . ?
C33 C30 C28 114.7(6) . . ?
F18 C30 C28 109.1(7) . . ?
F18 C30 C33 108.4(6) . . ?
C31 C32 C34 110(3) . . ?
F19 C32 C34 103.5(19) . . ?
F19 C32 C31 108.0(15) . . ?
F20 C32 C34 115.3(18) . . ?
F20 C32 C31 107.7(16) . . ?
F20 C32 F19 111.6(15) . . ?
C35 C33 C30 116.0(7) . . ?
F21 C33 C30 109.0(6) . . ?
F21 C33 C35 104.6(7) . . ?
F22 C33 C30 110.8(6) . . ?
F22 C33 C35 108.9(6) . . ?
F22 C33 F21 107.1(6) . . ?
F23 C34 C32 103(4) . . ?
F23 C34 F24 98(4) . . ?
F24 C34 C32 99(2) . . ?
F25 C34 C32 109(4) . . ?
F25 C34 F23 134(3) . . ?
F25 C34 F24 108(5) . . ?
F26 C35 C33 100(2) . . ?
F26 C35 F27 94.5(15) . . ?
F27 C35 C33 110.5(8) . . ?
F28 C35 C33 116.1(13) . . ?
F28 C35 F26 119.8(14) . . ?
F28 C35 F27 113.6(19) . . ?
C29 C31 F16 106(2) . . ?
C32 C31 C29 116(2) . . ?
C32 C31 F16 111(2) . . ?
F15 C31 C29 108(2) . . ?
F15 C31 C32 108(2) . . ?
F15 C31 F16 108(2) . . ?
C15 N1 C11 117.0(2) . . ?
C10 N2 C6 117.2(2) . . ?
C1 N3 C5 117.0(3) . . ?
C19 N4 H4A 116.4 . . ?
C22 N4 C19 127.2(3) . . ?
C22 N4 H4A 116.4 . . ?
Cl1 C36 H36 108.7 . . ?
Cl1 C36 Cl3 110.09(18) . . ?
Cl2 C36 H36 108.7 . . ?
Cl2 C36 Cl1 110.42(18) . . ?
Cl2 C36 Cl3 110.32(17) . . ?
Cl3 C36 H36 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.5(4) . . . . ?
C2 C1 N3 C5 0.0(4) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 C6 176.4(3) . . . . ?
C3 C4 C5 N3 -1.8(4) . . . . ?
C4 C5 C6 C7 -171.6(3) . . . . ?
C4 C5 C6 N2 8.1(4) . . . . ?
C4 C5 N3 C1 1.3(4) . . . . ?
C5 C6 C7 C8 -178.6(2) . . . . ?
C5 C6 N2 C10 179.5(2) . . . . ?
C6 C5 N3 C1 -176.9(2) . . . . ?
C6 C7 C8 C9 -1.2(4) . . . . ?
C6 C7 C8 C16 178.3(2) . . . . ?
C7 C6 N2 C10 -0.7(4) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C7 C8 C16 C17 168.9(3) . . . . ?
C7 C8 C16 C21 -11.8(4) . . . . ?
C8 C9 C10 C11 -179.7(2) . . . . ?
C8 C9 C10 N2 1.2(4) . . . . ?
C8 C16 C17 C18 178.6(3) . . . . ?
C8 C16 C21 C20 -179.3(3) . . . . ?
C9 C8 C16 C17 -11.7(4) . . . . ?
C9 C8 C16 C21 167.6(3) . . . . ?
C9 C10 C11 C12 167.6(2) . . . . ?
C9 C10 C11 N1 -12.7(4) . . . . ?
C9 C10 N2 C6 -0.7(4) . . . . ?
C10 C11 C12 C13 179.2(2) . . . . ?
C10 C11 N1 C15 -179.7(2) . . . . ?
C11 C10 N2 C6 -179.9(2) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C12 C11 N1 C15 0.0(4) . . . . ?
C12 C13 C14 C15 -0.4(4) . . . . ?
C13 C14 C15 N1 0.0(4) . . . . ?
C14 C15 N1 C11 0.2(4) . . . . ?
C16 C8 C9 C10 -179.6(2) . . . . ?
C16 C17 C18 C19 0.9(5) . . . . ?
C17 C16 C21 C20 0.0(4) . . . . ?
C17 C18 C19 C20 -0.5(4) . . . . ?
C17 C18 C19 N4 178.0(3) . . . . ?
C18 C19 C20 C21 -0.2(4) . . . . ?
C18 C19 N4 C22 2.7(4) . . . . ?
C19 C20 C21 C16 0.4(4) . . . . ?
C20 C19 N4 C22 -178.8(3) . . . . ?
C21 C16 C17 C18 -0.7(4) . . . . ?
C22 C23 C24 C27 177(2) . . . . ?
C22 C23 C24 F4 39.6(12) . . . . ?
C22 C23 C24 F6 -75.7(10) . . . . ?
C22 C23 C25 C26 168(3) . . . . ?
C22 C23 C25 F3 71(3) . . . . ?
C22 C23 C25 F5 -37(6) . . . . ?
C23 C22 N4 C19 -172.1(2) . . . . ?
C23 C24 C27 C29 -157(3) . . . . ?
C23 C24 C27 F8 -22(4) . . . . ?
C23 C24 C27 F10 83(2) . . . . ?
C23 C25 C26 C28 158(3) . . . . ?
C23 C25 C26 F7 -80(5) . . . . ?
C23 C25 C26 F9 33(5) . . . . ?
C24 C27 C29 F13 -36(4) . . . . ?
C24 C27 C29 F14 79(4) . . . . ?
C24 C27 C29 C31 -157(3) . . . . ?
C25 C26 C28 C30 167(3) . . . . ?
C25 C26 C28 F11 -73(3) . . . . ?
C25 C26 C28 F12 46(3) . . . . ?
C26 C28 C30 F17 46.7(12) . . . . ?
C26 C28 C30 C33 167.4(9) . . . . ?
C26 C28 C30 F18 -70.9(10) . . . . ?
C27 C29 C31 C32 -168(3) . . . . ?
C27 C29 C31 F15 71(3) . . . . ?
C27 C29 C31 F16 -44(3) . . . . ?
C28 C30 C33 C35 172.8(8) . . . . ?
C28 C30 C33 F21 55.2(10) . . . . ?
C28 C30 C33 F22 -62.3(8) . . . . ?
C30 C33 C35 F26 73.1(15) . . . . ?
C30 C33 C35 F27 171.6(8) . . . . ?
C30 C33 C35 F28 -57.2(13) . . . . ?
F17 C30 C33 C35 -65.4(10) . . . . ?
F17 C30 C33 F21 177.0(7) . . . . ?
F17 C30 C33 F22 59.5(8) . . . . ?
C34 C32 C31 C29 178.4(17) . . . . ?
C34 C32 C31 F15 -61(2) . . . . ?
C34 C32 C31 F16 58(2) . . . . ?
F1 C23 C24 C27 57(3) . . . . ?
F1 C23 C24 F4 -79.8(11) . . . . ?
F1 C23 C24 F6 165.0(7) . . . . ?
F1 C23 C25 C26 49(5) . . . . ?
F1 C23 C25 F3 -48(4) . . . . ?
F1 C23 C25 F5 -156(5) . . . . ?
F2 C23 C24 C27 -60(2) . . . . ?
F2 C23 C24 F4 162.9(9) . . . . ?
F2 C23 C24 F6 47.7(10) . . . . ?
F2 C23 C25 C26 -68(5) . . . . ?
F2 C23 C25 F3 -165(2) . . . . ?
F2 C23 C25 F5 87(5) . . . . ?
F3 C25 C26 C28 -90(2) . . . . ?
F3 C25 C26 F7 31.9(18) . . . . ?
F3 C25 C26 F9 145.0(14) . . . . ?
F4 C24 C27 C29 -22(4) . . . . ?
F4 C24 C27 F8 112(3) . . . . ?
F4 C24 C27 F10 -142.9(17) . . . . ?
F5 C25 C26 C28 0(5) . . . . ?
F5 C25 C26 F7 121(3) . . . . ?
F5 C25 C26 F9 -125(3) . . . . ?
F6 C24 C27 C29 94(4) . . . . ?
F6 C24 C27 F8 -131(3) . . . . ?
F6 C24 C27 F10 -26(2) . . . . ?
F7 C26 C28 C30 46.9(12) . . . . ?
F7 C26 C28 F11 166.7(7) . . . . ?
F7 C26 C28 F12 -74.9(11) . . . . ?
F8 C27 C29 F13 -166(3) . . . . ?
F8 C27 C29 F14 -51(4) . . . . ?
F8 C27 C29 C31 73(4) . . . . ?
F9 C26 C28 C30 -69.3(12) . . . . ?
F9 C26 C28 F11 50.5(10) . . . . ?
F9 C26 C28 F12 168.9(9) . . . . ?
F10 C27 C29 F13 76(4) . . . . ?
F10 C27 C29 F14 -169(3) . . . . ?
F10 C27 C29 C31 -46(4) . . . . ?
F11 C28 C30 F17 -72.4(8) . . . . ?
F11 C28 C30 C33 48.3(8) . . . . ?
F11 C28 C30 F18 170.0(5) . . . . ?
F12 C28 C30 F17 168.9(9) . . . . ?
F12 C28 C30 C33 -70.4(10) . . . . ?
F12 C28 C30 F18 51.4(9) . . . . ?
F13 C29 C31 C32 73(3) . . . . ?
F13 C29 C31 F15 -48(3) . . . . ?
F13 C29 C31 F16 -163(2) . . . . ?
F14 C29 C31 C32 -46(3) . . . . ?
F14 C29 C31 F15 -166.4(18) . . . . ?
F14 C29 C31 F16 78(2) . . . . ?
F18 C30 C33 C35 50.6(9) . . . . ?
F18 C30 C33 F21 -67.0(8) . . . . ?
F18 C30 C33 F22 175.4(5) . . . . ?
C31 C32 C34 F23 80(4) . . . . ?
C31 C32 C34 F24 -179.2(16) . . . . ?
C31 C32 C34 F25 -66(5) . . . . ?
F19 C32 C34 F23 -165(3) . . . . ?
F19 C32 C34 F24 -63.8(15) . . . . ?
F19 C32 C34 F25 49(5) . . . . ?
F19 C32 C31 C29 66(2) . . . . ?
F19 C32 C31 F15 -173.1(16) . . . . ?
F19 C32 C31 F16 -55(2) . . . . ?
F20 C32 C34 F23 -42(5) . . . . ?
F20 C32 C34 F24 58(2) . . . . ?
F20 C32 C34 F25 171(3) . . . . ?
F20 C32 C31 C29 -55(2) . . . . ?
F20 C32 C31 F15 66(2) . . . . ?
F20 C32 C31 F16 -175.6(16) . . . . ?
F21 C33 C35 F26 -166.9(13) . . . . ?
F21 C33 C35 F27 -68.3(10) . . . . ?
F21 C33 C35 F28 62.8(12) . . . . ?
F22 C33 C35 F26 -52.7(14) . . . . ?
F22 C33 C35 F27 45.8(10) . . . . ?
F22 C33 C35 F28 177.0(9) . . . . ?
N1 C11 C12 C13 -0.5(4) . . . . ?
N2 C6 C7 C8 1.7(4) . . . . ?
N2 C10 C11 C12 -13.2(4) . . . . ?
N2 C10 C11 N1 166.5(2) . . . . ?
N3 C1 C2 C3 -0.9(5) . . . . ?
N3 C5 C6 C7 6.7(4) . . . . ?
N3 C5 C6 N2 -173.6(2) . . . . ?
N4 C19 C20 C21 -178.7(3) . . . . ?
N4 C22 C23 C24 87.1(7) . . . . ?
N4 C22 C23 C25 88(3) . . . . ?
N4 C22 C23 F1 -153.3(3) . . . . ?
N4 C22 C23 F2 -34.6(3) . . . . ?
O1 C22 C23 C24 -90.5(7) . . . . ?
O1 C22 C23 C25 -90(3) . . . . ?
O1 C22 C23 F1 29.1(4) . . . . ?
O1 C22 C23 F2 147.9(3) . . . . ?
O1 C22 N4 C19 5.3(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2 16 4 0.0267 2.0042 16.0278 4.0020 0.2873 0.9555 -0.2092
-2 -14 -4 0.0248 -2.0041 -14.0277 -4.0018 -0.2978 -0.9412 0.1619
0 -35 3 0.0183 0.0001 -34.9886 2.9962 0.0819 0.2129 0.9896
0 33 -3 0.0223 -0.0002 32.9885 -2.9964 -0.0714 -0.2272 -0.9422
3 11 -4 0.0309 2.9993 10.9974 -3.9982 0.8374 -0.2026 -0.5427
-3 -2 4 0.0259 -2.9989 -1.9969 3.9992 -0.8846 0.2669 0.3296
1 -38 1 0.0155 0.9992 -37.9927 0.9961 0.4186 -0.0051 0.9307
0 -8 -6 0.0148 -0.0042 -8.0266 -6.0007 0.2449 -0.9830 -0.1325
0 21 5 0.0203 0.0042 21.0228 5.0021 -0.2792 0.9215 -0.2289
-1 -37 -2 0.0164 -1.0036 -37.0153 -2.0041 0.0083 -0.6849 0.7912
-1 -21 5 0.0187 -0.9983 -20.9839 4.9975 -0.3124 0.5095 0.7880

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3_CH3OH_H2O
_database_code_depnum_ccdc_archive 'CCDC 1533114'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT089_3.CH3OH.H2O         
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       4.74 Note  
RESPONSE: The data strategy was calculated and collected in triclinic
space group P-1, and later experiment is appended to reach completeness 99%
in non-centrosymmetric space group.
;
_vrf_PLAT340_3.CH3OH.H2O         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01385 Ang.  
RESPONSE: The data strategy was calculated and collected in triclinic
space group P-1, and later experiment is appended to reach completeness 99%
in non-centrosymmetric space group.
;
# end Validation Reply Form
_audit_creation_date             2017-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H15 F15 N4 O, C H4 O, H2 O'
_chemical_formula_sum            'C30 H21 F15 N4 O3'
_chemical_formula_weight         770.51
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C13 H14 N1 O4 F15'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 n 1'
_space_group_name_Hall           'P -2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   5.5175(6)
_cell_length_b                   31.498(3)
_cell_length_c                   9.0538(9)
_cell_angle_alpha                90
_cell_angle_beta                 99.363(10)
_cell_angle_gamma                90
_cell_volume                     1552.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2246
_cell_measurement_temperature    119.97(12)
_cell_measurement_theta_max      66.8820
_cell_measurement_theta_min      4.1810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.024
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22314
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.733
_diffrn_reflns_theta_max         66.733
_diffrn_reflns_theta_min         4.211
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.97(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -70.00   2.00    5.00    --  -41.90 -37.00-150.00   23
  2  ω    -70.00  30.00   2.00    5.00    --  -41.90  57.00 -90.00   50
  3  ω    -65.00  -9.00   2.00    5.00    --  -41.90 -77.00  90.00   28
  4  ω   -118.00 -10.00   2.00    5.00    --  -41.90 -77.00   0.00   54
  5  ω    -52.00 -14.00   2.00    5.00    --  -41.90 -57.00-180.00   19
  6  ω    -72.00 -18.00   2.00    5.00    --  -41.90 -37.00  60.00   27
  7  ω    -71.00 -13.00   2.00    5.00    --  -41.90 -77.00-180.00   29
  8  ω   -106.00 -78.00   2.00    5.00    --  -41.90 -77.00  90.00   14
  9  ω    -60.00 -20.00   2.00    5.00    --  -41.90 -37.00-150.00   20
 10  ω    -45.00  17.00   2.00    5.00    --  -41.90  42.00  27.00   31
 11  ω      1.00  83.00   2.00    5.00    --   41.90 -99.00  90.00   41
 12  ω     11.00  65.00   2.00    5.00    --   41.90  77.00 -60.00   27
 13  ω     75.00 117.00   2.00    5.00    --   41.90  77.00 -60.00   21
 14  ω     10.00  60.00   2.00    5.00    --   41.90  77.00  30.00   25
 15  ω     72.00 126.00   2.00   30.00    --  100.82  61.00 -60.00   27
 16  ω     73.00  99.00   2.00   30.00    --  100.82  61.00  60.00   13
 17  ω     68.00 176.00   2.00   30.00    --  100.82  77.00-120.00   54
 18  ω     95.00 171.00   2.00   30.00    --  100.82 125.00 -90.00   38
 19  ω     73.00 101.00   2.00   30.00    --  100.82  77.00 -60.00   14
 20  ω     70.00  96.00   2.00   30.00    --  100.82  71.00 -30.31   13
 21  ω     72.00 170.00   2.00   30.00    --  100.82  61.00  30.00   49
 22  ω     72.00 142.00   2.00   30.00    --  100.82  61.00-150.00   35
 23  ω     25.00 133.00   2.00   30.00    --  100.82 -77.00-120.00   54
 24  ω     73.00 115.00   2.00   30.00    --  100.82  61.00-180.00   21
 25  ω     69.00  97.00   2.00   30.00    --  100.82  77.00  90.00   14
 26  ω    140.00 174.00   2.00   30.00    --  100.82  77.00  90.00   17
 27  ω     68.00  96.00   2.00   30.00    --  100.82  77.00   0.00   14
 28  ω     69.00  95.00   2.00   30.00    --  100.82  77.00-180.00   13
 29  ω    109.00 173.00   2.00   30.00    --  100.82  63.00  77.28   32
 30  ω     68.00 134.00   2.00   30.00    --  100.82  77.00 120.00   33
 31  ω     72.00 100.00   2.00   30.00    --  100.82  61.00-120.00   14
 32  ω    139.00 167.00   2.00   30.00    --  100.82  61.00   0.00   14
 33  ω     18.00 108.00   2.00   30.00    --  100.82 -94.00-150.00   45
 34  ω     72.00 138.00   2.00   30.00    --  100.82  61.00   0.00   33
 35  ω     68.00  94.00   2.00   30.00    --  100.82  77.00 150.00   13
 36  ω     69.00  95.00   2.00   30.00    --  100.82  77.00  30.00   13
 37  ω    152.00 178.00   2.00   30.00    --  100.82  77.00  30.00   13
 38  ω     72.00 104.00   2.00   30.00    --  100.82  61.00  90.00   16
 39  ω     95.00 171.00   2.00   30.00    --  100.82 125.00 150.00   38
 40  ω    135.00 167.00   2.00   30.00    --  100.82  77.00 120.00   16
 41  ω     73.00 149.00   2.00   30.00    --  100.82  61.00 -30.00   38
 42  ω     72.00 100.00   2.00   30.00    --  100.82  61.00 120.00   14
 43  ω     28.00 122.00   2.00   30.00    --  100.82-125.00 120.00   47
 44  ω     71.00  97.00   2.00   30.00    --  100.82  63.00  77.28   13
 45  ω     69.00  95.00   2.00   30.00    --  100.82  73.00 137.46   13
 46  ω     69.00  95.00   2.00   30.00    --  100.82  74.00-103.45   13
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2257211000
_diffrn_orient_matrix_UB_12      -0.0169029000
_diffrn_orient_matrix_UB_13      0.0617320000
_diffrn_orient_matrix_UB_21      0.0995777000
_diffrn_orient_matrix_UB_22      0.0194682000
_diffrn_orient_matrix_UB_23      0.1541071000
_diffrn_orient_matrix_UB_31      -0.1383756000
_diffrn_orient_matrix_UB_32      0.0415596000
_diffrn_orient_matrix_UB_33      -0.0469583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3646
_reflns_number_total             5503
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 
;
 Flack x determined using 1249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.31(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         5503
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0618
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0615P)²+0.4509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1652
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9(4) 0.1(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(F10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F5)=Sof(F7)=1-FVAR(1)
 Sof(F6)=Sof(F8)=FVAR(1)
 Sof(F15)=Sof(F16)=1-FVAR(2)
 Sof(F13)=Sof(F14)=FVAR(2)
 Sof(F19)=Sof(F20)=Sof(C29)=1-FVAR(3)
 Sof(F17)=Sof(F18)=Sof(C28)=FVAR(3)
 Sof(F22)=Sof(F24)=Sof(F25)=1-FVAR(4)
 Sof(F21)=Sof(F23)=Sof(F26)=FVAR(4)
 Sof(F9)=Sof(F10)=1-FVAR(5)
 Sof(F11)=Sof(F12)=FVAR(5)
5.a Riding coordinates:
 O3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C3(H3), C4(H4A), C7(H7), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F -1.3669(9) -0.32286(18) -0.4321(6) 0.0658(14) Uani 1 1 d . . . . .
F2 F -1.3922(10) -0.31950(17) -0.1951(7) 0.0686(16) Uani 1 1 d . . . . .
F3 F -0.9747(13) -0.3672(2) -0.1328(7) 0.090(2) Uani 1 1 d . . . . .
F4 F -0.9535(11) -0.36973(17) -0.3692(8) 0.0807(19) Uani 1 1 d . . . . .
F5 F -1.278(2) -0.4145(5) -0.4605(14) 0.064(5) Uani 0.390(15) 1 d . . P A 2
F6 F -1.4542(17) -0.4035(3) -0.3947(14) 0.070(4) Uani 0.610(15) 1 d . . P A 1
F7 F -1.491(2) -0.3997(4) -0.2835(19) 0.056(5) Uani 0.390(15) 1 d . . P A 2
F8 F -1.369(2) -0.4059(3) -0.1468(12) 0.073(4) Uani 0.610(15) 1 d . . P A 1
F9 F -1.205(3) -0.4505(5) -0.0941(14) 0.050(5) Uani 0.334(15) 1 d . . P B 2
F10 F -0.930(8) -0.4451(13) -0.179(3) 0.055(7) Uani 0.334(15) 1 d . U P B 2
F11 F -0.923(3) -0.4510(6) -0.231(2) 0.058(4) Uani 0.666(15) 1 d . . P B 1
F12 F -1.0924(19) -0.4519(3) -0.4284(9) 0.077(3) Uani 0.666(15) 1 d . . P B 1
F13 F -1.3002(17) -0.4894(3) -0.1084(9) 0.065(3) Uani 0.646(17) 1 d . . P C 1
F14 F -1.534(4) -0.4877(7) -0.330(3) 0.041(3) Uani 0.646(17) 1 d . . P C 1
F15 F -1.495(9) -0.4787(14) -0.347(7) 0.054(8) Uani 0.354(17) 1 d . . P C 2
F16 F -1.205(3) -0.4971(5) -0.4434(13) 0.048(5) Uani 0.354(17) 1 d . . P C 2
F17 F -1.191(2) -0.5324(4) -0.4471(10) 0.077(4) Uani 0.618(16) 1 d . . P C 1
F18 F -0.9439(19) -0.5331(3) -0.2368(18) 0.067(3) Uani 0.618(16) 1 d . . P C 1
F19 F -0.988(3) -0.5315(5) -0.155(2) 0.057(5) Uani 0.382(16) 1 d . . P C 2
F20 F -1.362(3) -0.5307(6) -0.1046(15) 0.070(6) Uani 0.382(16) 1 d . . P C 2
F21 F -1.265(3) -0.5757(4) -0.1065(12) 0.096(5) Uani 0.588(18) 1 d . . P C 1
F22 F -1.137(3) -0.5812(5) -0.3960(18) 0.076(6) Uani 0.412(18) 1 d . . P C 2
F23 F -1.221(2) -0.6046(3) -0.3152(16) 0.083(4) Uani 0.588(18) 1 d . . P C 1
F24 F -1.268(3) -0.6054(5) -0.207(3) 0.089(7) Uani 0.412(18) 1 d . . P C 2
F25 F -1.510(3) -0.5717(5) -0.3780(18) 0.054(4) Uani 0.412(18) 1 d . . P C 2
F26 F -1.549(2) -0.5702(4) -0.294(2) 0.084(4) Uani 0.588(18) 1 d . . P C 1
O1 O -0.9911(13) -0.2714(2) -0.1450(8) 0.0724(19) Uani 1 1 d . . . . .
O2 O -1.1580(15) -0.2942(2) -0.6979(8) 0.077(2) Uani 1 1 d . . . . .
H2A H -1.1802 -0.2715 -0.7428 0.115 Uiso 1 1 calc GR . . . .
O3 O -1.1689(15) -0.2261(3) -0.9032(8) 0.084(2) Uani 1 1 d . . . . .
H3A H -1.0711 -0.2047 -0.8948 0.127 Uiso 1 1 d R . . . .
H3B H -1.1356 -0.2416 -0.9742 0.127 Uiso 1 1 d R . . . .
N1 N -0.0295(14) -0.0573(2) -0.1465(10) 0.062(2) Uani 1 1 d . . . . .
N2 N 0.1575(13) -0.0946(2) -0.4865(9) 0.0546(18) Uani 1 1 d . . . . .
N3 N 0.1439(16) -0.1502(3) -0.8397(9) 0.068(2) Uani 1 1 d . . . . .
N4 N -0.9561(13) -0.2759(2) -0.3950(8) 0.0520(17) Uani 1 1 d . . . . .
H4 H -1.0185 -0.2883 -0.4770 0.062 Uiso 1 1 calc R . . . .
C1 C 0.0381(18) -0.0276(3) -0.0417(14) 0.070(3) Uani 1 1 d . . . . .
H1 H -0.0587 -0.0246 0.0327 0.084 Uiso 1 1 calc R . . . .
C2 C 0.2388(19) -0.0014(3) -0.0351(14) 0.071(3) Uani 1 1 d . . . . .
H2 H 0.2719 0.0196 0.0377 0.086 Uiso 1 1 calc R . . . .
C3 C 0.3911(17) -0.0076(3) -0.1427(12) 0.063(3) Uani 1 1 d . . . . .
H3 H 0.5316 0.0088 -0.1415 0.076 Uiso 1 1 calc R . . . .
C4 C 0.3303(16) -0.0381(3) -0.2497(12) 0.059(2) Uani 1 1 d . . . . .
H4A H 0.4306 -0.0427 -0.3214 0.071 Uiso 1 1 calc R . . . .
C5 C 0.1194(15) -0.0624(3) -0.2520(10) 0.054(2) Uani 1 1 d . . . . .
C6 C 0.0457(16) -0.0950(3) -0.3638(10) 0.052(2) Uani 1 1 d . . . . .
C7 C -0.1334(16) -0.1250(3) -0.3467(10) 0.052(2) Uani 1 1 d . . . . .
H7 H -0.2098 -0.1240 -0.2624 0.063 Uiso 1 1 calc R . . . .
C8 C -0.1995(16) -0.1564(3) -0.4546(10) 0.054(2) Uani 1 1 d . . . . .
C9 C -0.0844(17) -0.1552(3) -0.5796(10) 0.058(2) Uani 1 1 d . . . . .
H9 H -0.1251 -0.1751 -0.6556 0.070 Uiso 1 1 calc R . . . .
C10 C 0.0909(17) -0.1246(3) -0.5918(11) 0.056(2) Uani 1 1 d . . . . .
C11 C 0.2182(17) -0.1227(3) -0.7254(12) 0.062(3) Uani 1 1 d . . . . .
C12 C 0.4095(19) -0.0938(3) -0.7295(13) 0.071(3) Uani 1 1 d . . . . .
H12 H 0.4559 -0.0751 -0.6504 0.086 Uiso 1 1 calc R . . . .
C13 C 0.530(2) -0.0933(4) -0.8533(14) 0.076(3) Uani 1 1 d . . . . .
H13 H 0.6583 -0.0744 -0.8581 0.091 Uiso 1 1 calc R . . . .
C14 C 0.456(2) -0.1213(4) -0.9684(13) 0.078(3) Uani 1 1 d . . . . .
H14 H 0.5328 -0.1216 -1.0524 0.093 Uiso 1 1 calc R . . . .
C15 C 0.264(2) -0.1492(4) -0.9578(12) 0.078(3) Uani 1 1 d . . . . .
H15 H 0.2157 -0.1681 -1.0361 0.093 Uiso 1 1 calc R . . . .
C16 C -0.3909(17) -0.1881(3) -0.4368(10) 0.056(2) Uani 1 1 d . . . . .
C17 C -0.5109(16) -0.2106(3) -0.5557(10) 0.060(2) Uani 1 1 d . . . . .
H17 H -0.4664 -0.2063 -0.6493 0.072 Uiso 1 1 calc R . . . .
C18 C -0.6987(15) -0.2399(3) -0.5429(10) 0.054(2) Uani 1 1 d . . . . .
H18 H -0.7768 -0.2548 -0.6257 0.065 Uiso 1 1 calc R . . . .
C19 C -0.7637(16) -0.2457(3) -0.4027(10) 0.052(2) Uani 1 1 d . . . . .
C20 C -0.636(2) -0.2260(3) -0.2779(11) 0.069(3) Uani 1 1 d . . . . .
H20 H -0.6725 -0.2316 -0.1831 0.083 Uiso 1 1 calc R . . . .
C21 C -0.450(2) -0.1975(3) -0.2979(11) 0.071(3) Uani 1 1 d . . . . .
H21 H -0.3625 -0.1842 -0.2140 0.085 Uiso 1 1 calc R . . . .
C22 C -1.0484(17) -0.2867(3) -0.2707(11) 0.055(2) Uani 1 1 d . . . . .
C23 C -1.2345(16) -0.3231(3) -0.2933(10) 0.055(2) Uani 1 1 d . . . . .
C24 C -1.1051(15) -0.3669(3) -0.2691(9) 0.051(2) Uani 1 1 d . . . . .
C25 C -1.2670(16) -0.4065(3) -0.2850(12) 0.060(2) Uani 1 1 d . . . . .
C26 C -1.1517(19) -0.4489(3) -0.2730(14) 0.072(3) Uani 1 1 d . . . . .
C27 C -1.2848(18) -0.4891(4) -0.2743(16) 0.074(3) Uani 1 1 d . . . . .
C28 C -1.182(3) -0.5312(5) -0.303(2) 0.055(4) Uani 0.618(16) 1 d . . P C 1
C29 C -1.223(5) -0.5319(8) -0.218(4) 0.052(7) Uani 0.382(16) 1 d . . P C 2
C30 C -1.301(2) -0.5713(4) -0.2700(17) 0.082(3) Uani 1 1 d . . . . .
C31 C -1.313(3) -0.3256(4) -0.7750(19) 0.116(5) Uani 1 1 d . . . . .
H31A H -1.2709 -0.3298 -0.8727 0.175 Uiso 1 1 calc GR . . . .
H31B H -1.4811 -0.3165 -0.7847 0.175 Uiso 1 1 calc GR . . . .
H31C H -1.2928 -0.3517 -0.7200 0.175 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C23 1.347(11) . ?
F2 C23 1.346(9) . ?
F3 C24 1.324(11) . ?
F4 C24 1.332(9) . ?
F5 C25 1.601(16) . ?
F6 C25 1.315(14) . ?
F7 C25 1.255(15) . ?
F8 C25 1.454(13) . ?
F9 C26 1.694(17) . ?
F10 C26 1.38(4) . ?
F11 C26 1.26(2) . ?
F12 C26 1.498(15) . ?
F13 C27 1.518(16) . ?
F14 C27 1.39(2) . ?
F15 C27 1.28(6) . ?
F16 C27 1.681(18) . ?
F17 C28 1.30(2) . ?
F18 C28 1.35(2) . ?
F19 C29 1.33(3) . ?
F20 C29 1.38(4) . ?
F21 C30 1.468(18) . ?
F22 C30 1.598(19) . ?
F23 C30 1.235(16) . ?
F24 C30 1.21(2) . ?
F25 C30 1.38(2) . ?
F26 C30 1.349(17) . ?
O1 C22 1.229(12) . ?
O2 H2A 0.8200 . ?
O2 C31 1.416(15) . ?
O3 H3A 0.8603 . ?
O3 H3B 0.8511 . ?
N1 C1 1.341(13) . ?
N1 C5 1.367(10) . ?
N2 C6 1.356(10) . ?
N2 C10 1.350(12) . ?
N3 C11 1.361(14) . ?
N3 C15 1.345(12) . ?
N4 H4 0.8600 . ?
N4 C19 1.435(11) . ?
N4 C22 1.351(11) . ?
C1 H1 0.9300 . ?
C1 C2 1.376(14) . ?
C2 H2 0.9300 . ?
C2 C3 1.401(13) . ?
C3 H3 0.9300 . ?
C3 C4 1.367(15) . ?
C4 H4A 0.9300 . ?
C4 C5 1.390(12) . ?
C5 C6 1.452(13) . ?
C6 C7 1.394(12) . ?
C7 H7 0.9300 . ?
C7 C8 1.397(13) . ?
C8 C9 1.385(11) . ?
C8 C16 1.482(13) . ?
C9 H9 0.9300 . ?
C9 C10 1.383(13) . ?
C10 C11 1.496(12) . ?
C11 C12 1.398(14) . ?
C12 H12 0.9300 . ?
C12 C13 1.394(13) . ?
C13 H13 0.9300 . ?
C13 C14 1.375(17) . ?
C14 H14 0.9300 . ?
C14 C15 1.392(17) . ?
C15 H15 0.9300 . ?
C16 C17 1.367(14) . ?
C16 C21 1.382(12) . ?
C17 H17 0.9300 . ?
C17 C18 1.406(13) . ?
C18 H18 0.9300 . ?
C18 C19 1.386(12) . ?
C19 C20 1.378(14) . ?
C20 H20 0.9300 . ?
C20 C21 1.398(14) . ?
C21 H21 0.9300 . ?
C22 C23 1.531(14) . ?
C23 C24 1.551(13) . ?
C24 C25 1.529(14) . ?
C25 C26 1.476(15) . ?
C26 C27 1.462(16) . ?
C27 C28 1.48(2) . ?
C27 C29 1.46(3) . ?
C28 C30 1.48(2) . ?
C29 C30 1.37(3) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C31 O2 H2A 109.5 . . ?
H3A O3 H3B 108.0 . . ?
C1 N1 C5 116.6(8) . . ?
C10 N2 C6 117.7(7) . . ?
C15 N3 C11 117.6(10) . . ?
C19 N4 H4 117.0 . . ?
C22 N4 H4 117.0 . . ?
C22 N4 C19 126.1(8) . . ?
N1 C1 H1 117.3 . . ?
N1 C1 C2 125.4(9) . . ?
C2 C1 H1 117.3 . . ?
C1 C2 H2 121.5 . . ?
C1 C2 C3 117.1(10) . . ?
C3 C2 H2 121.5 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.1(9) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4A 119.8 . . ?
C3 C4 C5 120.4(8) . . ?
C5 C4 H4A 119.8 . . ?
N1 C5 C4 121.4(9) . . ?
N1 C5 C6 116.0(7) . . ?
C4 C5 C6 122.5(7) . . ?
N2 C6 C5 116.9(7) . . ?
N2 C6 C7 121.5(8) . . ?
C7 C6 C5 121.6(7) . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.8(7) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C16 120.7(7) . . ?
C9 C8 C7 116.7(8) . . ?
C9 C8 C16 122.5(9) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(9) . . ?
C10 C9 H9 119.9 . . ?
N2 C10 C9 123.1(7) . . ?
N2 C10 C11 115.7(8) . . ?
C9 C10 C11 121.2(9) . . ?
N3 C11 C10 117.8(8) . . ?
N3 C11 C12 121.9(8) . . ?
C12 C11 C10 120.3(10) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 C11 119.4(12) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 H13 120.7 . . ?
C14 C13 C12 118.6(11) . . ?
C14 C13 H13 120.7 . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.3(9) . . ?
C15 C14 H14 120.4 . . ?
N3 C15 C14 123.2(12) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C17 C16 C8 121.8(7) . . ?
C17 C16 C21 116.8(9) . . ?
C21 C16 C8 121.4(9) . . ?
C16 C17 H17 118.5 . . ?
C16 C17 C18 123.0(8) . . ?
C18 C17 H17 118.5 . . ?
C17 C18 H18 121.1 . . ?
C19 C18 C17 117.8(9) . . ?
C19 C18 H18 121.1 . . ?
C18 C19 N4 115.9(8) . . ?
C20 C19 N4 122.8(8) . . ?
C20 C19 C18 121.2(8) . . ?
C19 C20 H20 120.9 . . ?
C19 C20 C21 118.1(8) . . ?
C21 C20 H20 120.9 . . ?
C16 C21 C20 122.8(10) . . ?
C16 C21 H21 118.6 . . ?
C20 C21 H21 118.6 . . ?
O1 C22 N4 126.7(9) . . ?
O1 C22 C23 118.9(7) . . ?
N4 C22 C23 114.4(8) . . ?
F1 C23 C22 111.7(7) . . ?
F1 C23 C24 107.7(7) . . ?
F2 C23 F1 107.8(7) . . ?
F2 C23 C22 109.9(7) . . ?
F2 C23 C24 108.3(7) . . ?
C22 C23 C24 111.4(7) . . ?
F3 C24 F4 109.1(8) . . ?
F3 C24 C23 107.8(7) . . ?
F3 C24 C25 107.6(8) . . ?
F4 C24 C23 106.9(7) . . ?
F4 C24 C25 107.6(7) . . ?
C25 C24 C23 117.7(7) . . ?
F6 C25 F8 106.4(9) . . ?
F6 C25 C24 112.8(8) . . ?
F6 C25 C26 113.4(10) . . ?
F7 C25 F5 99.2(12) . . ?
F7 C25 C24 114.8(10) . . ?
F7 C25 C26 124.6(11) . . ?
F8 C25 C24 102.2(9) . . ?
F8 C25 C26 99.9(8) . . ?
C24 C25 F5 98.5(7) . . ?
C26 C25 F5 82.9(9) . . ?
C26 C25 C24 119.6(7) . . ?
F10 C26 F9 71.8(16) . . ?
F10 C26 C25 107.2(18) . . ?
F10 C26 C27 118(2) . . ?
F11 C26 F12 85.4(11) . . ?
F11 C26 C25 117.8(12) . . ?
F11 C26 C27 115.8(12) . . ?
C25 C26 F9 87.5(8) . . ?
C25 C26 F12 98.3(9) . . ?
C27 C26 F9 79.5(9) . . ?
C27 C26 F12 97.2(9) . . ?
C27 C26 C25 125.0(8) . . ?
F14 C27 F13 98.5(13) . . ?
F14 C27 C26 116.2(12) . . ?
F14 C27 C28 110.6(15) . . ?
F15 C27 F16 85(3) . . ?
F15 C27 C26 101.2(19) . . ?
F15 C27 C29 124(2) . . ?
C26 C27 F13 96.1(9) . . ?
C26 C27 F16 86.1(9) . . ?
C26 C27 C28 124.8(11) . . ?
C28 C27 F13 104.6(11) . . ?
C29 C27 F16 95.7(18) . . ?
C29 C27 C26 134.9(12) . . ?
F17 C28 F18 108.4(16) . . ?
F17 C28 C27 104.3(13) . . ?
F17 C28 C30 103.4(14) . . ?
F18 C28 C27 109.6(14) . . ?
F18 C28 C30 107.8(12) . . ?
C30 C28 C27 122.5(15) . . ?
F19 C29 F20 108(3) . . ?
F19 C29 C27 107(2) . . ?
F19 C29 C30 113(2) . . ?
F20 C29 C27 96.2(19) . . ?
C30 C29 F20 96(2) . . ?
C30 C29 C27 132(2) . . ?
F21 C30 C28 106.9(12) . . ?
F23 C30 F21 104.9(12) . . ?
F23 C30 F26 112.3(13) . . ?
F23 C30 C28 117.7(14) . . ?
F24 C30 F22 95.7(16) . . ?
F24 C30 F25 111.6(14) . . ?
F24 C30 C29 129(2) . . ?
F25 C30 F22 89.8(12) . . ?
F26 C30 F21 97.6(14) . . ?
F26 C30 C28 114.6(12) . . ?
C29 C30 F22 103.8(18) . . ?
C29 C30 F25 115.5(15) . . ?
O2 C31 H31A 109.5 . . ?
O2 C31 H31B 109.5 . . ?
O2 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C23 C24 F3 179.9(7) . . . . ?
F1 C23 C24 F4 62.8(9) . . . . ?
F1 C23 C24 C25 -58.3(8) . . . . ?
F2 C23 C24 F3 -63.8(10) . . . . ?
F2 C23 C24 F4 179.1(8) . . . . ?
F2 C23 C24 C25 58.0(10) . . . . ?
F3 C24 C25 F5 -148.8(8) . . . . ?
F3 C24 C25 F6 160.6(9) . . . . ?
F3 C24 C25 F7 106.9(13) . . . . ?
F3 C24 C25 F8 46.8(9) . . . . ?
F3 C24 C25 C26 -62.1(10) . . . . ?
F4 C24 C25 F5 -31.4(10) . . . . ?
F4 C24 C25 F6 -82.0(11) . . . . ?
F4 C24 C25 F7 -135.7(12) . . . . ?
F4 C24 C25 F8 164.3(8) . . . . ?
F4 C24 C25 C26 55.3(11) . . . . ?
F5 C25 C26 F9 -164.6(9) . . . . ?
F5 C25 C26 F10 125.3(19) . . . . ?
F5 C25 C26 C27 -89.3(12) . . . . ?
F6 C25 C26 F11 146.0(14) . . . . ?
F6 C25 C26 F12 56.8(11) . . . . ?
F6 C25 C26 C27 -48.0(15) . . . . ?
F7 C25 C26 F9 -68.2(15) . . . . ?
F7 C25 C26 F10 -138(2) . . . . ?
F7 C25 C26 C27 7(2) . . . . ?
F8 C25 C26 F11 -101.3(15) . . . . ?
F8 C25 C26 F12 169.6(9) . . . . ?
F8 C25 C26 C27 64.8(13) . . . . ?
F9 C26 C27 F15 105(3) . . . . ?
F9 C26 C27 F16 -170.4(9) . . . . ?
F9 C26 C27 C29 -76(3) . . . . ?
F10 C26 C27 F15 168(3) . . . . ?
F10 C26 C27 F16 -107.8(17) . . . . ?
F10 C26 C27 C29 -14(3) . . . . ?
F11 C26 C27 F13 81.5(14) . . . . ?
F11 C26 C27 F14 -175.9(18) . . . . ?
F11 C26 C27 C28 -31(2) . . . . ?
F12 C26 C27 F13 169.9(8) . . . . ?
F12 C26 C27 F14 -87.5(17) . . . . ?
F12 C26 C27 C28 57.5(15) . . . . ?
F13 C27 C28 F17 174.2(12) . . . . ?
F13 C27 C28 F18 -69.9(16) . . . . ?
F13 C27 C28 C30 57.7(16) . . . . ?
F14 C27 C28 F17 69.1(18) . . . . ?
F14 C27 C28 F18 -175.0(16) . . . . ?
F14 C27 C28 C30 -47(2) . . . . ?
F15 C27 C29 F19 177(4) . . . . ?
F15 C27 C29 F20 -72(4) . . . . ?
F15 C27 C29 C30 31(5) . . . . ?
F16 C27 C29 F19 89(2) . . . . ?
F16 C27 C29 F20 -160.4(15) . . . . ?
F16 C27 C29 C30 -57(3) . . . . ?
F17 C28 C30 F21 171.4(12) . . . . ?
F17 C28 C30 F23 53.8(17) . . . . ?
F17 C28 C30 F26 -81.6(18) . . . . ?
F18 C28 C30 F21 56.8(18) . . . . ?
F18 C28 C30 F23 -61(2) . . . . ?
F18 C28 C30 F26 163.8(18) . . . . ?
F19 C29 C30 F22 -62(3) . . . . ?
F19 C29 C30 F24 47(4) . . . . ?
F19 C29 C30 F25 -159(2) . . . . ?
F20 C29 C30 F22 -174.6(14) . . . . ?
F20 C29 C30 F24 -66(3) . . . . ?
F20 C29 C30 F25 89(2) . . . . ?
O1 C22 C23 F1 149.7(8) . . . . ?
O1 C22 C23 F2 30.1(12) . . . . ?
O1 C22 C23 C24 -89.9(9) . . . . ?
N1 C1 C2 C3 -3.2(18) . . . . ?
N1 C5 C6 N2 166.2(8) . . . . ?
N1 C5 C6 C7 -13.1(13) . . . . ?
N2 C6 C7 C8 1.5(14) . . . . ?
N2 C10 C11 N3 -175.1(9) . . . . ?
N2 C10 C11 C12 5.9(13) . . . . ?
N3 C11 C12 C13 -0.6(16) . . . . ?
N4 C19 C20 C21 179.3(9) . . . . ?
N4 C22 C23 F1 -32.9(10) . . . . ?
N4 C22 C23 F2 -152.5(8) . . . . ?
N4 C22 C23 C24 87.5(9) . . . . ?
C1 N1 C5 C4 0.2(14) . . . . ?
C1 N1 C5 C6 179.3(9) . . . . ?
C1 C2 C3 C4 1.8(17) . . . . ?
C2 C3 C4 C5 0.4(15) . . . . ?
C3 C4 C5 N1 -1.5(14) . . . . ?
C3 C4 C5 C6 179.5(9) . . . . ?
C4 C5 C6 N2 -14.7(13) . . . . ?
C4 C5 C6 C7 165.9(9) . . . . ?
C5 N1 C1 C2 2.2(17) . . . . ?
C5 C6 C7 C8 -179.1(8) . . . . ?
C6 N2 C10 C9 0.0(13) . . . . ?
C6 N2 C10 C11 179.6(8) . . . . ?
C6 C7 C8 C9 -2.0(14) . . . . ?
C6 C7 C8 C16 -179.7(8) . . . . ?
C7 C8 C9 C10 1.5(14) . . . . ?
C7 C8 C16 C17 160.1(9) . . . . ?
C7 C8 C16 C21 -22.3(14) . . . . ?
C8 C9 C10 N2 -0.5(14) . . . . ?
C8 C9 C10 C11 179.9(9) . . . . ?
C8 C16 C17 C18 -177.9(8) . . . . ?
C8 C16 C21 C20 177.5(10) . . . . ?
C9 C8 C16 C17 -17.5(15) . . . . ?
C9 C8 C16 C21 160.2(10) . . . . ?
C9 C10 C11 N3 4.5(14) . . . . ?
C9 C10 C11 C12 -174.4(9) . . . . ?
C10 N2 C6 C5 -179.9(8) . . . . ?
C10 N2 C6 C7 -0.5(12) . . . . ?
C10 C11 C12 C13 178.3(9) . . . . ?
C11 N3 C15 C14 -0.7(17) . . . . ?
C11 C12 C13 C14 0.2(17) . . . . ?
C12 C13 C14 C15 -0.1(17) . . . . ?
C13 C14 C15 N3 0.4(18) . . . . ?
C15 N3 C11 C10 -178.1(9) . . . . ?
C15 N3 C11 C12 0.8(16) . . . . ?
C16 C8 C9 C10 179.1(9) . . . . ?
C16 C17 C18 C19 0.3(14) . . . . ?
C17 C16 C21 C20 -4.8(16) . . . . ?
C17 C18 C19 N4 -180.0(8) . . . . ?
C17 C18 C19 C20 -5.0(13) . . . . ?
C18 C19 C20 C21 4.6(15) . . . . ?
C19 N4 C22 O1 3.1(15) . . . . ?
C19 N4 C22 C23 -174.0(8) . . . . ?
C19 C20 C21 C16 0.4(17) . . . . ?
C21 C16 C17 C18 4.4(14) . . . . ?
C22 N4 C19 C18 179.9(8) . . . . ?
C22 N4 C19 C20 4.9(13) . . . . ?
C22 C23 C24 F3 57.1(8) . . . . ?
C22 C23 C24 F4 -60.0(9) . . . . ?
C22 C23 C24 C25 178.9(7) . . . . ?
C23 C24 C25 F5 89.3(9) . . . . ?
C23 C24 C25 F6 38.7(12) . . . . ?
C23 C24 C25 F7 -15.1(14) . . . . ?
C23 C24 C25 F8 -75.1(9) . . . . ?
C23 C24 C25 C26 176.0(8) . . . . ?
C24 C25 C26 F9 99.6(10) . . . . ?
C24 C25 C26 F10 30(2) . . . . ?
C24 C25 C26 F11 9.0(17) . . . . ?
C24 C25 C26 F12 -80.2(9) . . . . ?
C24 C25 C26 C27 175.0(10) . . . . ?
C25 C26 C27 F13 -84.7(11) . . . . ?
C25 C26 C27 F14 18(2) . . . . ?
C25 C26 C27 F15 26(3) . . . . ?
C25 C26 C27 F16 110.2(12) . . . . ?
C25 C26 C27 C28 162.9(13) . . . . ?
C25 C26 C27 C29 -156(2) . . . . ?
C26 C27 C28 F17 -77.5(17) . . . . ?
C26 C27 C28 F18 38(2) . . . . ?
C26 C27 C28 C30 166.0(13) . . . . ?
C26 C27 C29 F19 -2(4) . . . . ?
C26 C27 C29 F20 109(2) . . . . ?
C26 C27 C29 C30 -147(2) . . . . ?
C27 C28 C30 F21 -71.6(16) . . . . ?
C27 C28 C30 F23 170.8(15) . . . . ?
C27 C28 C30 F26 35(2) . . . . ?
C27 C29 C30 F22 82(3) . . . . ?
C27 C29 C30 F24 -169(3) . . . . ?
C27 C29 C30 F25 -15(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.692
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9(4)
2 0.1(4)

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1533110'
_audit_update_record             
;
2017-02-16 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT089_3                   
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       5.52 Note  
RESPONSE: The data strategy was calculated and collected in triclinic
space group P-1, and later experiment is appended to reach completeness 99%
in non-centrosymmetric space group.  
;
# end Validation Reply Form
_audit_creation_date             2017-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H15 F15 N4 O'
_chemical_formula_sum            'C29 H15 F15 N4 O'
_chemical_formula_weight         720.45
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 N4 F15'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   9.78405(18)
_cell_length_b                   10.07442(18)
_cell_length_c                   55.2622(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5447.12(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    28130
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      74.0710
_cell_measurement_theta_min      4.6510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75971
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -36 0.0071
0 0 36 0.0165
-5 4 -1 0.1189
-6 0 2 0.0921
5 -4 -4 0.0771
4 5 2 0.0706
1 6 3 0.0645
-2 -6 -3 0.0746

_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.024
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0026 -0.0047 -35.9910 -0.5232 0.8509 0.0968
0.0026 0.0047 35.9910 0.5232 -0.8509 -0.0968
-4.9985 4.0000 -0.9934 -0.0586 0.1092 -0.9895
-5.9979 0.0002 2.0083 0.4898 0.3204 -0.7434
4.9982 -4.0007 -4.0054 -0.0141 0.0090 1.0029
3.9988 5.0006 1.9925 -0.8131 -0.5683 0.0152
0.9998 6.0007 2.9964 -0.6752 -0.4633 -0.4508
-1.9995 -6.0007 -2.9949 0.7520 0.5246 0.3278

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            82852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.746
_diffrn_reflns_theta_max         66.746
_diffrn_reflns_theta_min         4.389
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  21.00   1.00    4.00    --  -41.90  57.00  60.00   90
  2  ω   -122.00  -1.00   1.00    4.00    --  -41.90 -19.00 -90.00  121
  3  ω   -101.00 -76.00   1.00    4.00    --  -41.90-149.00  98.00   25
  4  ω     14.00 118.00   1.00    4.00    --   41.90  77.00  30.00  104
  5  ω     69.00 116.00   1.00    4.00    --   41.90  37.00 120.00   47
  6  ω      9.00  94.00   1.00    4.00    --   41.90  77.00 -30.00   85
  7  ω     23.00  95.00   1.00    4.00    --   41.90-125.00-180.00   72
  8  ω     13.00  87.00   1.00    4.00    --   41.90  77.00-180.00   74
  9  ω     10.00  55.00   1.00    4.00    --   41.90  77.00  90.00   45
 10  ω      2.00  58.00   1.00    4.00    --   41.90 -99.00 -60.00   56
 11  ω     14.00  64.00   1.00    4.00    --   41.90  57.00 150.00   50
 12  ω     10.00 108.00   1.00    4.00    --   41.90  77.00-120.00   98
 13  ω     72.00 114.00   1.00    4.00    --   41.90  57.00 150.00   42
 14  ω     18.00  61.00   1.00    4.00    --   41.90  37.00 120.00   43
 15  ω     74.00 100.00   1.00   16.00    --  106.66  77.00 -60.00   26
 16  ω     25.00 102.00   1.00   16.00    --  106.66 -94.00 -60.00   77
 17  ω    107.00 177.00   1.00   16.00    --  106.66  71.00 -76.71   70
 18  ω     78.00 110.00   1.00   16.00    --  106.66  60.00-110.78   32
 19  ω     78.00 104.00   1.00   16.00    --  106.66  60.00-138.88   26
 20  ω     76.00 102.00   1.00   16.00    --  106.66  71.00 -76.71   26
 21  ω     78.00 108.00   1.00   16.00    --  106.66  60.00-116.45   30
 22  ω    109.00 178.00   1.00   16.00    --  106.66  77.00  30.00   69
 23  ω     78.00 104.00   1.00   16.00    --  106.66  61.00  90.00   26
 24  ω     78.00 139.00   1.00   16.00    --  106.66  61.00 -90.00   61
 25  ω     79.00 106.00   1.00   16.00    --  106.66  61.00 -30.00   27
 26  ω    107.00 149.00   1.00   16.00    --  106.66  61.00 -30.00   42
 27  ω     74.00 146.00   1.00   16.00    --  106.66  77.00 150.00   72
 28  ω     78.00 105.00   1.00   16.00    --  106.66  61.00  60.00   27
 29  ω     74.00  99.00   1.00   16.00    --  106.66  77.00  30.00   25
 30  ω     79.00 104.00   1.00   16.00    --  106.66  61.00-180.00   25
 31  ω     78.00 104.00   1.00   16.00    --  106.66  61.00 122.14   26
 32  ω     53.00  80.00   1.00   16.00    --  106.66-125.00-150.00   27
 33  ω     74.00 100.00   1.00   16.00    --  106.66  77.00-150.00   26
 34  ω     77.00 149.00   1.00   16.00    --  106.66  65.00 -16.30   72
 35  ω     77.00 103.00   1.00   16.00    --  106.66  63.00 127.47   26
 36  ω     74.00 178.00   1.00   16.00    --  106.66  77.00-180.00  104
 37  ω     34.00 108.00   1.00   16.00    --  106.66 -94.00  30.00   74
 38  ω     24.00 105.00   1.00   16.00    --  106.66 -94.00-150.00   81
 39  ω     77.00 107.00   1.00   16.00    --  106.66  65.00  28.95   30
 40  ω    116.00 178.00   1.00   16.00    --  106.66  77.00-150.00   62
 41  ω     74.00 144.00   1.00   16.00    --  106.66  77.00  60.00   70
 42  ω     97.00 122.00   1.00   16.00    --  106.66-125.00-150.00   25
 43  ω     78.00 104.00   1.00   16.00    --  106.66  61.00-150.00   26
 44  ω    114.00 178.00   1.00   16.00    --  106.66  77.00   0.00   64
 45  ω     74.00 177.00   1.00   16.00    --  106.66  77.00  90.00  103
 46  ω     74.00 100.00   1.00   16.00    --  106.66  77.00   0.00   26
 47  ω     79.00 139.00   1.00   16.00    --  106.66  61.00 150.00   60
 48  ω     74.00 100.00   1.00   16.00    --  106.66  77.00 120.00   26
 49  ω    115.00 178.00   1.00   16.00    --  106.66  77.00 120.00   63
 50  ω     74.00 100.00   1.00   16.00    --  106.66  77.00-120.00   26
 51  ω     24.00 102.00   1.00   16.00    --  106.66 -94.00 120.00   78
 52  ω     80.00 106.00   1.00   16.00    --  106.66  47.00 -57.19   26
 53  ω    124.00 149.00   1.00   16.00    --  106.66  60.00-116.45   25
 54  ω     78.00 104.00   1.00   16.00    --  106.66  58.00   6.86   26
 55  ω     78.00 104.00   1.00   16.00    --  106.66  58.00 -50.55   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0767846000
_diffrn_orient_matrix_UB_12      -0.1069902000
_diffrn_orient_matrix_UB_13      0.0145560000
_diffrn_orient_matrix_UB_21      -0.0613256000
_diffrn_orient_matrix_UB_22      -0.0551971000
_diffrn_orient_matrix_UB_23      -0.0236310000
_diffrn_orient_matrix_UB_31      0.1230332000
_diffrn_orient_matrix_UB_32      -0.0942847000
_diffrn_orient_matrix_UB_33      -0.0026849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8985
_reflns_number_total             9628
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 
;
 Flack x determined using 4105 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0522P)²+1.8624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0954
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N4A(H4AA), C1(H1), C1A(H1A), C2(H2), C2A(H2A), C3(H3), C3A(H3A),
 C4(H4A), C4A(H4AB), C7(H7), C7A(H7A), C9(H9), C9A(H9A), C12(H12), C12A(H12A),
 C13(H13), C13A(H13A), C14(H14), C14A(H14A), C15(H15), C15A(H15A), C17(H17),
 C17A(H17A), C18(H18), C18A(H18A), C20(H20), C20A(H20A), C21(H21), C21A(H21A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.0590(2) -0.1222(2) 0.43906(4) 0.0222(4) Uani 1 1 d . . . . .
F1A F 0.6839(2) 0.3775(2) 0.56070(4) 0.0226(5) Uani 1 1 d . . . . .
F2 F 0.2823(2) -0.1263(2) 0.43801(4) 0.0231(4) Uani 1 1 d . . . . .
F2A F 0.4606(2) 0.3736(2) 0.56179(4) 0.0227(5) Uani 1 1 d . . . . .
F3 F 0.0654(2) 0.1141(2) 0.46314(4) 0.0244(5) Uani 1 1 d . . . . .
F3A F 0.6777(2) 0.6138(2) 0.53654(4) 0.0239(5) Uani 1 1 d . . . . .
F4 F 0.2882(2) 0.1163(2) 0.46098(4) 0.0269(5) Uani 1 1 d . . . . .
F4A F 0.4550(2) 0.6159(2) 0.53874(4) 0.0259(5) Uani 1 1 d . . . . .
F5 F 0.0736(2) -0.1217(2) 0.48762(4) 0.0268(5) Uani 1 1 d . . . . .
F5A F 0.6697(2) 0.3789(2) 0.51213(4) 0.0265(5) Uani 1 1 d . . . . .
F6 F 0.2960(2) -0.1210(2) 0.48577(4) 0.0302(5) Uani 1 1 d . . . . .
F6A F 0.4470(2) 0.3785(2) 0.51404(4) 0.0295(5) Uani 1 1 d . . . . .
F7 F 0.0772(2) 0.1172(2) 0.51095(4) 0.0272(5) Uani 1 1 d . . . . .
F7A F 0.6657(2) 0.6174(2) 0.48885(4) 0.0269(5) Uani 1 1 d . . . . .
F8 F 0.2997(2) 0.1226(2) 0.50870(4) 0.0302(5) Uani 1 1 d . . . . .
F8A F 0.4431(3) 0.6224(2) 0.49113(4) 0.0305(5) Uani 1 1 d . . . . .
F9 F 0.0883(2) -0.1160(2) 0.53564(4) 0.0276(5) Uani 1 1 d . . . . .
F9A F 0.4326(2) 0.3826(2) 0.46695(4) 0.0296(5) Uani 1 1 d . . . . .
F10 F 0.3106(2) -0.1176(2) 0.53275(4) 0.0300(5) Uani 1 1 d . . . . .
F10A F 0.6552(2) 0.3837(2) 0.46417(4) 0.0279(5) Uani 1 1 d . . . . .
F11 F 0.0992(3) 0.1240(2) 0.55898(4) 0.0304(5) Uani 1 1 d . . . . .
F11A F 0.4221(3) 0.6222(2) 0.44351(4) 0.0320(5) Uani 1 1 d . . . . .
F12 F 0.3216(3) 0.1223(2) 0.55629(4) 0.0322(5) Uani 1 1 d . . . . .
F12A F 0.6445(2) 0.6236(2) 0.44077(4) 0.0290(5) Uani 1 1 d . . . . .
F13 F 0.2399(3) 0.0456(3) 0.59931(4) 0.0370(6) Uani 1 1 d . . . . .
F13A F 0.4223(3) 0.3790(3) 0.41962(4) 0.0400(6) Uani 1 1 d . . . . .
F14 F 0.1041(3) -0.1015(3) 0.58486(4) 0.0436(7) Uani 1 1 d . . . . .
F14A F 0.6396(3) 0.3972(3) 0.41502(4) 0.0418(6) Uani 1 1 d . . . . .
F15 F 0.3205(3) -0.1221(3) 0.58001(4) 0.0391(6) Uani 1 1 d . . . . .
F15A F 0.5046(3) 0.5458(3) 0.40040(4) 0.0367(6) Uani 1 1 d . . . . .
O1 O 0.0549(2) 0.0925(2) 0.41080(4) 0.0205(5) Uani 1 1 d . . . . .
O1A O 0.6882(2) 0.5918(3) 0.58903(4) 0.0203(5) Uani 1 1 d . . . . .
N1 N 0.2885(3) 0.8439(3) 0.33575(6) 0.0254(7) Uani 1 1 d . . . . .
N1A N 0.0165(3) 0.8721(3) 0.71980(6) 0.0224(7) Uani 1 1 d . . . . .
N2 N 0.5436(3) 0.6514(3) 0.30444(5) 0.0191(6) Uani 1 1 d . . . . .
N2A N 0.1984(3) 1.1516(3) 0.69513(5) 0.0191(6) Uani 1 1 d . . . . .
N3 N 0.7140(4) 0.3780(4) 0.27625(7) 0.0285(8) Uani 1 1 d . . . . .
N3A N 0.4517(3) 1.3475(3) 0.66376(6) 0.0238(7) Uani 1 1 d . . . . .
N4 N 0.2865(3) 0.0653(3) 0.40546(6) 0.0183(6) Uani 1 1 d . . . . .
H4 H 0.3530 0.0161 0.4102 0.022 Uiso 1 1 calc R . . . .
N4A N 0.4570(3) 0.5655(3) 0.59431(5) 0.0177(6) Uani 1 1 d . . . . .
H4AA H 0.3902 0.5166 0.5896 0.021 Uiso 1 1 calc R . . . .
C1 C 0.2367(4) 0.9674(4) 0.33546(8) 0.0264(8) Uani 1 1 d . . . . .
H1 H 0.1648 0.9871 0.3459 0.032 Uiso 1 1 calc R . . . .
C1A C -0.0775(4) 0.8483(4) 0.73687(7) 0.0264(8) Uani 1 1 d . . . . .
H1A H -0.1043 0.7609 0.7395 0.032 Uiso 1 1 calc R . . . .
C2 C 0.2854(4) 1.0675(4) 0.32035(7) 0.0252(8) Uani 1 1 d . . . . .
H2 H 0.2481 1.1524 0.3208 0.030 Uiso 1 1 calc R . . . .
C2A C -0.1372(4) 0.9465(4) 0.75088(7) 0.0248(8) Uani 1 1 d . . . . .
H2A H -0.2014 0.9254 0.7627 0.030 Uiso 1 1 calc R . . . .
C3 C 0.3908(4) 1.0370(4) 0.30468(7) 0.0259(8) Uani 1 1 d . . . . .
H3 H 0.4261 1.1015 0.2944 0.031 Uiso 1 1 calc R . . . .
C3A C -0.0992(5) 1.0752(5) 0.74694(8) 0.0319(10) Uani 1 1 d . . . . .
H3A H -0.1357 1.1432 0.7563 0.038 Uiso 1 1 calc R . . . .
C4 C 0.4432(4) 0.9100(4) 0.30444(7) 0.0240(8) Uani 1 1 d . . . . .
H4A H 0.5128 0.8875 0.2937 0.029 Uiso 1 1 calc R . . . .
C4A C -0.0059(4) 1.1034(4) 0.72885(8) 0.0284(9) Uani 1 1 d . . . . .
H4AB H 0.0190 1.1907 0.7256 0.034 Uiso 1 1 calc R . . . .
C5 C 0.3909(4) 0.8152(3) 0.32044(6) 0.0194(7) Uani 1 1 d . . . . .
C5A C 0.0503(4) 0.9992(3) 0.71564(9) 0.0181(10) Uani 1 1 d . . . . .
C6 C 0.4452(4) 0.6778(4) 0.32071(6) 0.0194(7) Uani 1 1 d . . . . .
C6A C 0.1534(4) 1.0259(4) 0.69648(7) 0.0181(7) Uani 1 1 d . . . . .
C7 C 0.3947(4) 0.5821(4) 0.33681(6) 0.0193(7) Uani 1 1 d . . . . .
H7 H 0.3278 0.6043 0.3480 0.023 Uiso 1 1 calc R . . . .
C7A C 0.1992(3) 0.9254(3) 0.68119(6) 0.0170(7) Uani 1 1 d . . . . .
H7A H 0.1651 0.8396 0.6827 0.020 Uiso 1 1 calc R . . . .
C8 C 0.4459(4) 0.4535(4) 0.33579(7) 0.0181(7) Uani 1 1 d . . . . .
C8A C 0.2973(4) 0.9553(4) 0.66354(6) 0.0178(7) Uani 1 1 d . . . . .
C9 C 0.5453(4) 0.4252(4) 0.31828(6) 0.0197(7) Uani 1 1 d . . . . .
H9 H 0.5803 0.3398 0.3168 0.024 Uiso 1 1 calc R . . . .
C9A C 0.3454(4) 1.0858(4) 0.66243(7) 0.0181(7) Uani 1 1 d . . . . .
H9A H 0.4102 1.1097 0.6509 0.022 Uiso 1 1 calc R . . . .
C10 C 0.5909(4) 0.5260(4) 0.30325(7) 0.0188(7) Uani 1 1 d . . . . .
C10A C 0.2957(3) 1.1798(3) 0.67863(6) 0.0174(7) Uani 1 1 d . . . . .
C11 C 0.6979(5) 0.5029(3) 0.28432(9) 0.0197(10) Uani 1 1 d . . . . .
C11A C 0.3492(3) 1.3192(3) 0.67925(6) 0.0185(7) Uani 1 1 d . . . . .
C12 C 0.7758(4) 0.6081(4) 0.27585(7) 0.0256(9) Uani 1 1 d . . . . .
H12 H 0.7629 0.6931 0.2820 0.031 Uiso 1 1 calc R . . . .
C12A C 0.2971(4) 1.4115(4) 0.69543(7) 0.0225(8) Uani 1 1 d . . . . .
H12A H 0.2266 1.3884 0.7059 0.027 Uiso 1 1 calc R . . . .
C13 C 0.8732(4) 0.5852(5) 0.25807(8) 0.0311(9) Uani 1 1 d . . . . .
H13 H 0.9265 0.6544 0.2521 0.037 Uiso 1 1 calc R . . . .
C13A C 0.3514(4) 1.5390(4) 0.69578(7) 0.0250(8) Uani 1 1 d . . . . .
H13A H 0.3174 1.6026 0.7064 0.030 Uiso 1 1 calc R . . . .
C14 C 0.8893(4) 0.4578(5) 0.24943(8) 0.0310(9) Uani 1 1 d . . . . .
H14 H 0.9526 0.4392 0.2373 0.037 Uiso 1 1 calc R . . . .
C14A C 0.4569(4) 1.5697(4) 0.68006(7) 0.0248(8) Uani 1 1 d . . . . .
H14A H 0.4960 1.6538 0.6799 0.030 Uiso 1 1 calc R . . . .
C15 C 0.8097(4) 0.3594(4) 0.25912(8) 0.0333(9) Uani 1 1 d . . . . .
H15 H 0.8228 0.2734 0.2534 0.040 Uiso 1 1 calc R . . . .
C15A C 0.5019(4) 1.4713(4) 0.66474(8) 0.0262(8) Uani 1 1 d . . . . .
H15A H 0.5728 1.4924 0.6542 0.031 Uiso 1 1 calc R . . . .
C16 C 0.3991(4) 0.3491(3) 0.35291(6) 0.0176(7) Uani 1 1 d . . . . .
C16A C 0.3452(4) 0.8520(3) 0.64646(6) 0.0179(7) Uani 1 1 d . . . . .
C17 C 0.2652(4) 0.3461(3) 0.36156(6) 0.0191(7) Uani 1 1 d . . . . .
H17 H 0.2030 0.4092 0.3561 0.023 Uiso 1 1 calc R . . . .
C17A C 0.2545(4) 0.7536(4) 0.63860(6) 0.0195(7) Uani 1 1 d . . . . .
H17A H 0.1658 0.7521 0.6446 0.023 Uiso 1 1 calc R . . . .
C18 C 0.2225(4) 0.2508(3) 0.37814(6) 0.0191(7) Uani 1 1 d . . . . .
H18 H 0.1323 0.2489 0.3834 0.023 Uiso 1 1 calc R . . . .
C18A C 0.2948(4) 0.6590(4) 0.62206(6) 0.0197(7) Uani 1 1 d . . . . .
H18A H 0.2330 0.5946 0.6170 0.024 Uiso 1 1 calc R . . . .
C19 C 0.3165(4) 0.1582(3) 0.38677(6) 0.0175(7) Uani 1 1 d . . . . .
C19A C 0.4277(3) 0.6592(3) 0.61290(6) 0.0166(6) Uani 1 1 d . . . . .
C20 C 0.4492(4) 0.1577(4) 0.37771(6) 0.0194(7) Uani 1 1 d . . . . .
H20 H 0.5107 0.0931 0.3828 0.023 Uiso 1 1 calc R . . . .
C20A C 0.5216(4) 0.7524(3) 0.62127(6) 0.0193(7) Uani 1 1 d . . . . .
H20A H 0.6118 0.7504 0.6159 0.023 Uiso 1 1 calc R . . . .
C21 C 0.4905(3) 0.2528(3) 0.36116(6) 0.0195(7) Uani 1 1 d . . . . .
H21 H 0.5800 0.2525 0.3555 0.023 Uiso 1 1 calc R . . . .
C21A C 0.4789(3) 0.8486(3) 0.63770(6) 0.0190(7) Uani 1 1 d . . . . .
H21A H 0.5410 0.9123 0.6430 0.023 Uiso 1 1 calc R . . . .
C22 C 0.1658(4) 0.0464(4) 0.41638(6) 0.0166(7) Uani 1 1 d . . . . .
C22A C 0.5776(3) 0.5456(4) 0.58346(6) 0.0166(7) Uani 1 1 d . . . . .
C23 C 0.1723(4) -0.0459(4) 0.43889(7) 0.0174(7) Uani 1 1 d . . . . .
C23A C 0.5708(3) 0.4540(4) 0.56091(7) 0.0176(7) Uani 1 1 d . . . . .
C24 C 0.1779(4) 0.0371(4) 0.46261(7) 0.0169(7) Uani 1 1 d . . . . .
C24A C 0.5657(4) 0.5375(4) 0.53725(7) 0.0170(7) Uani 1 1 d . . . . .
C25 C 0.1850(4) -0.0433(4) 0.48648(7) 0.0172(7) Uani 1 1 d . . . . .
C25A C 0.5579(4) 0.4557(4) 0.51331(7) 0.0177(7) Uani 1 1 d . . . . .
C26 C 0.1909(4) 0.0426(4) 0.50994(7) 0.0183(7) Uani 1 1 d . . . . .
C26A C 0.5523(4) 0.5422(4) 0.48983(7) 0.0176(7) Uani 1 1 d . . . . .
C27 C 0.1999(4) -0.0390(4) 0.53380(7) 0.0188(7) Uani 1 1 d . . . . .
C27A C 0.5428(4) 0.4607(4) 0.46594(7) 0.0177(7) Uani 1 1 d . . . . .
C28 C 0.2106(4) 0.0458(4) 0.55724(7) 0.0205(7) Uani 1 1 d . . . . .
C28A C 0.5340(4) 0.5462(4) 0.44253(7) 0.0203(7) Uani 1 1 d . . . . .
C29 C 0.2189(4) -0.0359(5) 0.58075(7) 0.0248(8) Uani 1 1 d . . . . .
C29A C 0.5250(4) 0.4630(5) 0.41882(7) 0.0248(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C23 1.349(4) . ?
F1A C23A 1.348(4) . ?
F2 C23 1.349(4) . ?
F2A C23A 1.350(4) . ?
F3 C24 1.347(4) . ?
F3A C24A 1.339(4) . ?
F4 C24 1.345(4) . ?
F4A C24A 1.343(4) . ?
F5 C25 1.347(4) . ?
F5A C25A 1.342(4) . ?
F6 C25 1.339(4) . ?
F6A C25A 1.335(4) . ?
F7 C26 1.344(4) . ?
F7A C26A 1.345(4) . ?
F8 C26 1.337(4) . ?
F8A C26A 1.341(4) . ?
F9 C27 1.344(4) . ?
F9A C27A 1.336(4) . ?
F10 C27 1.343(4) . ?
F10A C27A 1.350(4) . ?
F11 C28 1.348(4) . ?
F11A C28A 1.337(4) . ?
F12 C28 1.333(5) . ?
F12A C28A 1.337(4) . ?
F13 C29 1.330(5) . ?
F13A C29A 1.314(5) . ?
F14 C29 1.323(5) . ?
F14A C29A 1.319(5) . ?
F15 C29 1.320(5) . ?
F15A C29A 1.331(5) . ?
O1 C22 1.220(4) . ?
O1A C22A 1.217(4) . ?
N1 C1 1.343(5) . ?
N1 C5 1.343(5) . ?
N1A C1A 1.339(5) . ?
N1A C5A 1.342(5) . ?
N2 C6 1.344(5) . ?
N2 C10 1.346(5) . ?
N2A C6A 1.343(5) . ?
N2A C10A 1.349(4) . ?
N3 C11 1.344(5) . ?
N3 C15 1.345(6) . ?
N3A C11A 1.349(5) . ?
N3A C15A 1.342(5) . ?
N4 H4 0.8600 . ?
N4 C19 1.424(4) . ?
N4 C22 1.340(5) . ?
N4A H4AA 0.8600 . ?
N4A C19A 1.424(4) . ?
N4A C22A 1.339(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.393(6) . ?
C1A H1A 0.9300 . ?
C1A C2A 1.385(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(6) . ?
C2A H2A 0.9300 . ?
C2A C3A 1.366(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(6) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.383(6) . ?
C4 H4A 0.9300 . ?
C4 C5 1.399(5) . ?
C4A H4AB 0.9300 . ?
C4A C5A 1.392(6) . ?
C5 C6 1.482(5) . ?
C5A C6A 1.487(6) . ?
C6 C7 1.402(5) . ?
C6A C7A 1.393(5) . ?
C7 H7 0.9300 . ?
C7 C8 1.390(6) . ?
C7A H7A 0.9300 . ?
C7A C8A 1.401(5) . ?
C8 C9 1.401(5) . ?
C8 C16 1.486(5) . ?
C8A C9A 1.398(5) . ?
C8A C16A 1.481(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.385(6) . ?
C9A H9A 0.9300 . ?
C9A C10A 1.391(5) . ?
C10 C11 1.498(6) . ?
C10A C11A 1.499(5) . ?
C11 C12 1.387(6) . ?
C11A C12A 1.387(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.388(6) . ?
C12A H12A 0.9300 . ?
C12A C13A 1.390(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.378(7) . ?
C13A H13A 0.9300 . ?
C13A C14A 1.385(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.370(6) . ?
C14A H14A 0.9300 . ?
C14A C15A 1.375(6) . ?
C15 H15 0.9300 . ?
C15A H15A 0.9300 . ?
C16 C17 1.395(5) . ?
C16 C21 1.396(5) . ?
C16A C17A 1.399(5) . ?
C16A C21A 1.395(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.391(5) . ?
C17A H17A 0.9300 . ?
C17A C18A 1.379(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.394(5) . ?
C18A H18A 0.9300 . ?
C18A C19A 1.396(5) . ?
C19 C20 1.392(5) . ?
C19A C20A 1.393(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.385(5) . ?
C20A H20A 0.9300 . ?
C20A C21A 1.393(5) . ?
C21 H21 0.9300 . ?
C21A H21A 0.9300 . ?
C22 C23 1.554(5) . ?
C22A C23A 1.552(5) . ?
C23 C24 1.556(5) . ?
C23A C24A 1.555(5) . ?
C24 C25 1.549(5) . ?
C24A C25A 1.561(5) . ?
C25 C26 1.560(5) . ?
C25A C26A 1.564(5) . ?
C26 C27 1.556(5) . ?
C26A C27A 1.557(5) . ?
C27 C28 1.555(5) . ?
C27A C28A 1.557(5) . ?
C28 C29 1.541(5) . ?
C28A C29A 1.558(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 N1 C1 118.3(3) . . ?
C1A N1A C5A 117.4(4) . . ?
C6 N2 C10 117.7(3) . . ?
C6A N2A C10A 117.9(3) . . ?
C11 N3 C15 116.5(4) . . ?
C15A N3A C11A 116.3(3) . . ?
C19 N4 H4 116.5 . . ?
C22 N4 H4 116.5 . . ?
C22 N4 C19 127.0(3) . . ?
C19A N4A H4AA 116.6 . . ?
C22A N4A H4AA 116.6 . . ?
C22A N4A C19A 126.8(3) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(4) . . ?
C2 C1 H1 118.4 . . ?
N1A C1A H1A 118.1 . . ?
N1A C1A C2A 123.7(4) . . ?
C2A C1A H1A 118.1 . . ?
C1 C2 H2 121.0 . . ?
C3 C2 C1 118.0(4) . . ?
C3 C2 H2 121.0 . . ?
C1A C2A H2A 120.8 . . ?
C3A C2A C1A 118.3(4) . . ?
C3A C2A H2A 120.8 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(4) . . ?
C4 C3 H3 120.3 . . ?
C2A C3A H3A 120.4 . . ?
C2A C3A C4A 119.3(4) . . ?
C4A C3A H3A 120.4 . . ?
C3 C4 H4A 120.3 . . ?
C3 C4 C5 119.5(4) . . ?
C5 C4 H4A 120.3 . . ?
C3A C4A H4AB 120.5 . . ?
C3A C4A C5A 119.0(4) . . ?
C5A C4A H4AB 120.5 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 117.6(3) . . ?
C4 C5 C6 120.8(3) . . ?
N1A C5A C4A 122.2(4) . . ?
N1A C5A C6A 117.5(4) . . ?
C4A C5A C6A 120.3(3) . . ?
N2 C6 C5 115.8(3) . . ?
N2 C6 C7 122.7(3) . . ?
C7 C6 C5 121.5(3) . . ?
N2A C6A C5A 115.6(3) . . ?
N2A C6A C7A 123.1(4) . . ?
C7A C6A C5A 121.2(3) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.3(3) . . ?
C8 C7 H7 120.4 . . ?
C6A C7A H7A 120.4 . . ?
C6A C7A C8A 119.1(3) . . ?
C8A C7A H7A 120.4 . . ?
C7 C8 C9 117.8(3) . . ?
C7 C8 C16 121.5(3) . . ?
C9 C8 C16 120.7(3) . . ?
C7A C8A C16A 120.6(3) . . ?
C9A C8A C7A 117.6(3) . . ?
C9A C8A C16A 121.8(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.2(3) . . ?
C10 C9 H9 120.4 . . ?
C8A C9A H9A 120.2 . . ?
C10A C9A C8A 119.6(3) . . ?
C10A C9A H9A 120.2 . . ?
N2 C10 C9 123.2(4) . . ?
N2 C10 C11 114.8(3) . . ?
C9 C10 C11 121.9(4) . . ?
N2A C10A C9A 122.6(3) . . ?
N2A C10A C11A 115.4(3) . . ?
C9A C10A C11A 122.0(3) . . ?
N3 C11 C10 117.3(4) . . ?
N3 C11 C12 122.6(4) . . ?
C12 C11 C10 120.1(4) . . ?
N3A C11A C10A 116.3(3) . . ?
N3A C11A C12A 122.7(3) . . ?
C12A C11A C10A 120.9(3) . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.3(4) . . ?
C13 C12 H12 120.4 . . ?
C11A C12A H12A 120.4 . . ?
C11A C12A C13A 119.2(4) . . ?
C13A C12A H12A 120.4 . . ?
C12 C13 H13 120.7 . . ?
C14 C13 C12 118.6(4) . . ?
C14 C13 H13 120.7 . . ?
C12A C13A H13A 120.6 . . ?
C14A C13A C12A 118.9(4) . . ?
C14A C13A H13A 120.6 . . ?
C13 C14 H14 120.9 . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 H14 120.9 . . ?
C13A C14A H14A 121.2 . . ?
C15A C14A C13A 117.6(4) . . ?
C15A C14A H14A 121.2 . . ?
N3 C15 C14 124.8(4) . . ?
N3 C15 H15 117.6 . . ?
C14 C15 H15 117.6 . . ?
N3A C15A C14A 125.3(4) . . ?
N3A C15A H15A 117.3 . . ?
C14A C15A H15A 117.3 . . ?
C17 C16 C8 121.5(3) . . ?
C17 C16 C21 118.3(3) . . ?
C21 C16 C8 120.1(3) . . ?
C17A C16A C8A 119.7(3) . . ?
C21A C16A C8A 122.3(3) . . ?
C21A C16A C17A 118.0(3) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.5(3) . . ?
C18 C17 H17 119.2 . . ?
C16A C17A H17A 119.5 . . ?
C18A C17A C16A 121.0(3) . . ?
C18A C17A H17A 119.5 . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.3(3) . . ?
C19 C18 H18 120.3 . . ?
C17A C18A H18A 119.8 . . ?
C17A C18A C19A 120.4(3) . . ?
C19A C18A H18A 119.8 . . ?
C18 C19 N4 123.5(3) . . ?
C20 C19 N4 116.8(3) . . ?
C20 C19 C18 119.6(3) . . ?
C18A C19A N4A 116.6(3) . . ?
C20A C19A N4A 123.6(3) . . ?
C20A C19A C18A 119.7(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.5(3) . . ?
C21 C20 H20 119.8 . . ?
C19A C20A H20A 120.4 . . ?
C19A C20A C21A 119.2(3) . . ?
C21A C20A H20A 120.4 . . ?
C16 C21 H21 119.7 . . ?
C20 C21 C16 120.6(3) . . ?
C20 C21 H21 119.7 . . ?
C16A C21A H21A 119.2 . . ?
C20A C21A C16A 121.6(3) . . ?
C20A C21A H21A 119.2 . . ?
O1 C22 N4 128.0(3) . . ?
O1 C22 C23 117.8(3) . . ?
N4 C22 C23 114.2(3) . . ?
O1A C22A N4A 127.8(3) . . ?
O1A C22A C23A 117.9(3) . . ?
N4A C22A C23A 114.2(3) . . ?
F1 C23 F2 108.3(3) . . ?
F1 C23 C22 108.2(3) . . ?
F1 C23 C24 109.2(3) . . ?
F2 C23 C22 111.3(3) . . ?
F2 C23 C24 109.0(3) . . ?
C22 C23 C24 110.8(3) . . ?
F1A C23A F2A 108.2(3) . . ?
F1A C23A C22A 108.2(3) . . ?
F1A C23A C24A 109.2(3) . . ?
F2A C23A C22A 111.2(3) . . ?
F2A C23A C24A 109.2(3) . . ?
C22A C23A C24A 110.8(3) . . ?
F3 C24 C23 107.4(3) . . ?
F3 C24 C25 108.6(3) . . ?
F4 C24 F3 108.4(3) . . ?
F4 C24 C23 106.9(3) . . ?
F4 C24 C25 109.3(3) . . ?
C25 C24 C23 116.0(3) . . ?
F3A C24A F4A 108.9(3) . . ?
F3A C24A C23A 108.0(3) . . ?
F3A C24A C25A 108.6(3) . . ?
F4A C24A C23A 107.0(3) . . ?
F4A C24A C25A 108.9(3) . . ?
C23A C24A C25A 115.4(3) . . ?
F5 C25 C24 108.1(3) . . ?
F5 C25 C26 108.4(3) . . ?
F6 C25 F5 108.4(3) . . ?
F6 C25 C24 108.5(3) . . ?
F6 C25 C26 108.6(3) . . ?
C24 C25 C26 114.8(3) . . ?
F5A C25A C24A 107.8(3) . . ?
F5A C25A C26A 108.0(3) . . ?
F6A C25A F5A 109.2(3) . . ?
F6A C25A C24A 108.8(3) . . ?
F6A C25A C26A 108.7(3) . . ?
C24A C25A C26A 114.3(3) . . ?
F7 C26 C25 108.3(3) . . ?
F7 C26 C27 107.9(3) . . ?
F8 C26 F7 108.9(3) . . ?
F8 C26 C25 108.7(3) . . ?
F8 C26 C27 108.4(3) . . ?
C27 C26 C25 114.4(3) . . ?
F7A C26A C25A 108.6(3) . . ?
F7A C26A C27A 108.2(3) . . ?
F8A C26A F7A 108.6(3) . . ?
F8A C26A C25A 108.6(3) . . ?
F8A C26A C27A 108.4(3) . . ?
C27A C26A C25A 114.3(3) . . ?
F9 C27 C26 108.8(3) . . ?
F9 C27 C28 108.0(3) . . ?
F10 C27 F9 108.5(3) . . ?
F10 C27 C26 108.7(3) . . ?
F10 C27 C28 107.8(3) . . ?
C28 C27 C26 114.8(3) . . ?
F9A C27A F10A 108.8(3) . . ?
F9A C27A C26A 108.9(3) . . ?
F9A C27A C28A 108.4(3) . . ?
F10A C27A C26A 108.4(3) . . ?
F10A C27A C28A 107.6(3) . . ?
C28A C27A C26A 114.6(3) . . ?
F11 C28 C27 109.0(3) . . ?
F11 C28 C29 107.1(3) . . ?
F12 C28 F11 108.9(3) . . ?
F12 C28 C27 109.8(3) . . ?
F12 C28 C29 107.4(3) . . ?
C29 C28 C27 114.4(4) . . ?
F11A C28A C27A 109.2(3) . . ?
F11A C28A C29A 107.2(3) . . ?
F12A C28A F11A 109.3(3) . . ?
F12A C28A C27A 109.8(3) . . ?
F12A C28A C29A 107.4(3) . . ?
C27A C28A C29A 113.9(4) . . ?
F13 C29 C28 109.2(4) . . ?
F14 C29 F13 107.9(3) . . ?
F14 C29 C28 111.5(3) . . ?
F15 C29 F13 108.3(3) . . ?
F15 C29 F14 108.4(4) . . ?
F15 C29 C28 111.4(3) . . ?
F13A C29A F14A 109.4(4) . . ?
F13A C29A F15A 108.3(3) . . ?
F13A C29A C28A 111.2(3) . . ?
F14A C29A F15A 108.7(3) . . ?
F14A C29A C28A 110.9(3) . . ?
F15A C29A C28A 108.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C23 C24 F3 -60.6(4) . . . . ?
F1 C23 C24 F4 -176.8(3) . . . . ?
F1 C23 C24 C25 61.0(4) . . . . ?
F1A C23A C24A F3A -60.3(4) . . . . ?
F1A C23A C24A F4A -177.4(3) . . . . ?
F1A C23A C24A C25A 61.3(4) . . . . ?
F2 C23 C24 F3 -178.8(3) . . . . ?
F2 C23 C24 F4 65.1(4) . . . . ?
F2 C23 C24 C25 -57.1(4) . . . . ?
F2A C23A C24A F3A -178.5(3) . . . . ?
F2A C23A C24A F4A 64.5(4) . . . . ?
F2A C23A C24A C25A -56.8(4) . . . . ?
F3 C24 C25 F5 61.9(4) . . . . ?
F3 C24 C25 F6 179.2(3) . . . . ?
F3 C24 C25 C26 -59.2(4) . . . . ?
F3A C24A C25A F5A 61.2(4) . . . . ?
F3A C24A C25A F6A 179.4(3) . . . . ?
F3A C24A C25A C26A -58.9(4) . . . . ?
F4 C24 C25 F5 -180.0(3) . . . . ?
F4 C24 C25 F6 -62.7(4) . . . . ?
F4 C24 C25 C26 58.9(4) . . . . ?
F4A C24A C25A F5A 179.6(3) . . . . ?
F4A C24A C25A F6A -62.1(4) . . . . ?
F4A C24A C25A C26A 59.5(4) . . . . ?
F5 C25 C26 F7 -60.5(4) . . . . ?
F5 C25 C26 F8 -178.8(3) . . . . ?
F5 C25 C26 C27 59.8(4) . . . . ?
F5A C25A C26A F7A -60.2(4) . . . . ?
F5A C25A C26A F8A -178.1(3) . . . . ?
F5A C25A C26A C27A 60.7(4) . . . . ?
F6 C25 C26 F7 -178.0(3) . . . . ?
F6 C25 C26 F8 63.7(4) . . . . ?
F6 C25 C26 C27 -57.7(4) . . . . ?
F6A C25A C26A F7A -178.5(3) . . . . ?
F6A C25A C26A F8A 63.5(4) . . . . ?
F6A C25A C26A C27A -57.6(4) . . . . ?
F7 C26 C27 F9 59.8(4) . . . . ?
F7 C26 C27 F10 177.9(3) . . . . ?
F7 C26 C27 C28 -61.3(4) . . . . ?
F7A C26A C27A F9A 178.2(3) . . . . ?
F7A C26A C27A F10A 60.0(4) . . . . ?
F7A C26A C27A C28A -60.2(4) . . . . ?
F8 C26 C27 F9 177.7(3) . . . . ?
F8 C26 C27 F10 -64.3(4) . . . . ?
F8 C26 C27 C28 56.6(4) . . . . ?
F8A C26A C27A F9A -64.1(4) . . . . ?
F8A C26A C27A F10A 177.7(3) . . . . ?
F8A C26A C27A C28A 57.5(4) . . . . ?
F9 C27 C28 F11 -61.7(4) . . . . ?
F9 C27 C28 F12 179.0(3) . . . . ?
F9 C27 C28 C29 58.2(4) . . . . ?
F9A C27A C28A F11A 61.4(4) . . . . ?
F9A C27A C28A F12A -178.8(3) . . . . ?
F9A C27A C28A C29A -58.4(4) . . . . ?
F10 C27 C28 F11 -178.8(3) . . . . ?
F10 C27 C28 F12 61.9(4) . . . . ?
F10 C27 C28 C29 -58.9(4) . . . . ?
F10A C27A C28A F11A 179.0(3) . . . . ?
F10A C27A C28A F12A -61.2(4) . . . . ?
F10A C27A C28A C29A 59.2(4) . . . . ?
F11 C28 C29 F13 -64.5(4) . . . . ?
F11 C28 C29 F14 54.6(5) . . . . ?
F11 C28 C29 F15 175.8(3) . . . . ?
F11A C28A C29A F13A -65.8(4) . . . . ?
F11A C28A C29A F14A 172.3(3) . . . . ?
F11A C28A C29A F15A 53.1(4) . . . . ?
F12 C28 C29 F13 52.3(4) . . . . ?
F12 C28 C29 F14 171.4(3) . . . . ?
F12 C28 C29 F15 -67.3(4) . . . . ?
F12A C28A C29A F13A 176.9(3) . . . . ?
F12A C28A C29A F14A 55.0(4) . . . . ?
F12A C28A C29A F15A -64.2(4) . . . . ?
O1 C22 C23 F1 38.4(4) . . . . ?
O1 C22 C23 F2 157.3(3) . . . . ?
O1 C22 C23 C24 -81.3(4) . . . . ?
O1A C22A C23A F1A 38.7(4) . . . . ?
O1A C22A C23A F2A 157.5(3) . . . . ?
O1A C22A C23A C24A -80.8(4) . . . . ?
N1 C1 C2 C3 1.0(6) . . . . ?
N1 C5 C6 N2 177.3(3) . . . . ?
N1 C5 C6 C7 -1.8(5) . . . . ?
N1A C1A C2A C3A 0.7(6) . . . . ?
N1A C5A C6A N2A -171.1(4) . . . . ?
N1A C5A C6A C7A 8.7(6) . . . . ?
N2 C6 C7 C8 -1.2(5) . . . . ?
N2 C10 C11 N3 -156.9(4) . . . . ?
N2 C10 C11 C12 23.2(6) . . . . ?
N2A C6A C7A C8A 0.3(6) . . . . ?
N2A C10A C11A N3A 176.6(3) . . . . ?
N2A C10A C11A C12A -1.9(5) . . . . ?
N3 C11 C12 C13 1.0(7) . . . . ?
N3A C11A C12A C13A 0.3(6) . . . . ?
N4 C19 C20 C21 -174.0(3) . . . . ?
N4 C22 C23 F1 -141.7(3) . . . . ?
N4 C22 C23 F2 -22.8(4) . . . . ?
N4 C22 C23 C24 98.5(3) . . . . ?
N4A C19A C20A C21A 173.3(3) . . . . ?
N4A C22A C23A F1A -142.2(3) . . . . ?
N4A C22A C23A F2A -23.5(4) . . . . ?
N4A C22A C23A C24A 98.2(3) . . . . ?
C1 N1 C5 C4 -0.2(5) . . . . ?
C1 N1 C5 C6 -179.0(3) . . . . ?
C1 C2 C3 C4 0.3(6) . . . . ?
C1A N1A C5A C4A 2.0(6) . . . . ?
C1A N1A C5A C6A -179.3(4) . . . . ?
C1A C2A C3A C4A 1.6(6) . . . . ?
C2 C3 C4 C5 -1.4(6) . . . . ?
C2A C3A C4A C5A -2.0(7) . . . . ?
C3 C4 C5 N1 1.4(6) . . . . ?
C3 C4 C5 C6 -179.8(3) . . . . ?
C3A C4A C5A N1A 0.2(7) . . . . ?
C3A C4A C5A C6A -178.5(4) . . . . ?
C4 C5 C6 N2 -1.5(5) . . . . ?
C4 C5 C6 C7 179.3(3) . . . . ?
C4A C5A C6A N2A 7.7(6) . . . . ?
C4A C5A C6A C7A -172.5(4) . . . . ?
C5 N1 C1 C2 -1.1(6) . . . . ?
C5 C6 C7 C8 177.9(3) . . . . ?
C5A N1A C1A C2A -2.5(6) . . . . ?
C5A C6A C7A C8A -179.5(4) . . . . ?
C6 N2 C10 C9 -1.5(5) . . . . ?
C6 N2 C10 C11 178.6(3) . . . . ?
C6 C7 C8 C9 -0.9(5) . . . . ?
C6 C7 C8 C16 178.1(3) . . . . ?
C6A N2A C10A C9A 3.2(5) . . . . ?
C6A N2A C10A C11A -175.5(3) . . . . ?
C6A C7A C8A C9A 0.6(5) . . . . ?
C6A C7A C8A C16A -178.0(3) . . . . ?
C7 C8 C9 C10 1.7(5) . . . . ?
C7 C8 C16 C17 33.7(5) . . . . ?
C7 C8 C16 C21 -144.9(4) . . . . ?
C7A C8A C9A C10A 0.3(5) . . . . ?
C7A C8A C16A C17A 33.6(5) . . . . ?
C7A C8A C16A C21A -146.5(3) . . . . ?
C8 C9 C10 N2 -0.5(6) . . . . ?
C8 C9 C10 C11 179.4(4) . . . . ?
C8 C16 C17 C18 -178.0(3) . . . . ?
C8 C16 C21 C20 177.9(3) . . . . ?
C8A C9A C10A N2A -2.3(5) . . . . ?
C8A C9A C10A C11A 176.4(3) . . . . ?
C8A C16A C17A C18A 177.7(3) . . . . ?
C8A C16A C21A C20A -178.7(3) . . . . ?
C9 C8 C16 C17 -147.3(3) . . . . ?
C9 C8 C16 C21 34.1(5) . . . . ?
C9 C10 C11 N3 23.3(6) . . . . ?
C9 C10 C11 C12 -156.7(4) . . . . ?
C9A C8A C16A C17A -145.0(4) . . . . ?
C9A C8A C16A C21A 34.9(5) . . . . ?
C9A C10A C11A N3A -2.1(5) . . . . ?
C9A C10A C11A C12A 179.4(3) . . . . ?
C10 N2 C6 C5 -176.7(3) . . . . ?
C10 N2 C6 C7 2.4(5) . . . . ?
C10 C11 C12 C13 -179.1(4) . . . . ?
C10A N2A C6A C5A 177.6(3) . . . . ?
C10A N2A C6A C7A -2.2(5) . . . . ?
C10A C11A C12A C13A 178.7(3) . . . . ?
C11 N3 C15 C14 -0.6(7) . . . . ?
C11 C12 C13 C14 -0.1(6) . . . . ?
C11A N3A C15A C14A -0.3(6) . . . . ?
C11A C12A C13A C14A -0.5(6) . . . . ?
C12 C13 C14 C15 -1.1(6) . . . . ?
C12A C13A C14A C15A 0.4(6) . . . . ?
C13 C14 C15 N3 1.5(7) . . . . ?
C13A C14A C15A N3A 0.0(7) . . . . ?
C15 N3 C11 C10 179.5(4) . . . . ?
C15 N3 C11 C12 -0.6(6) . . . . ?
C15A N3A C11A C10A -178.4(3) . . . . ?
C15A N3A C11A C12A 0.1(5) . . . . ?
C16 C8 C9 C10 -177.3(3) . . . . ?
C16 C17 C18 C19 1.6(5) . . . . ?
C16A C8A C9A C10A 178.9(3) . . . . ?
C16A C17A C18A C19A 0.3(5) . . . . ?
C17 C16 C21 C20 -0.7(5) . . . . ?
C17 C18 C19 N4 173.6(3) . . . . ?
C17 C18 C19 C20 -3.5(5) . . . . ?
C17A C16A C21A C20A 1.2(5) . . . . ?
C17A C18A C19A N4A -174.5(3) . . . . ?
C17A C18A C19A C20A 2.6(5) . . . . ?
C18 C19 C20 C21 3.4(5) . . . . ?
C18A C19A C20A C21A -3.5(5) . . . . ?
C19 N4 C22 O1 9.4(6) . . . . ?
C19 N4 C22 C23 -170.4(3) . . . . ?
C19 C20 C21 C16 -1.2(5) . . . . ?
C19A N4A C22A O1A 9.1(6) . . . . ?
C19A N4A C22A C23A -169.9(3) . . . . ?
C19A C20A C21A C16A 1.7(5) . . . . ?
C21 C16 C17 C18 0.5(5) . . . . ?
C21A C16A C17A C18A -2.2(5) . . . . ?
C22 N4 C19 C18 4.3(5) . . . . ?
C22 N4 C19 C20 -178.4(3) . . . . ?
C22 C23 C24 F3 58.5(3) . . . . ?
C22 C23 C24 F4 -57.7(4) . . . . ?
C22 C23 C24 C25 -179.9(3) . . . . ?
C22A N4A C19A C18A -177.9(3) . . . . ?
C22A N4A C19A C20A 5.1(5) . . . . ?
C22A C23A C24A F3A 58.7(3) . . . . ?
C22A C23A C24A F4A -58.4(3) . . . . ?
C22A C23A C24A C25A -179.7(3) . . . . ?
C23 C24 C25 F5 -59.0(4) . . . . ?
C23 C24 C25 F6 58.3(4) . . . . ?
C23 C24 C25 C26 179.9(3) . . . . ?
C23A C24A C25A F5A -60.1(4) . . . . ?
C23A C24A C25A F6A 58.1(4) . . . . ?
C23A C24A C25A C26A 179.8(3) . . . . ?
C24 C25 C26 F7 60.4(4) . . . . ?
C24 C25 C26 F8 -57.8(4) . . . . ?
C24 C25 C26 C27 -179.2(3) . . . . ?
C24A C25A C26A F7A 59.8(4) . . . . ?
C24A C25A C26A F8A -58.1(4) . . . . ?
C24A C25A C26A C27A -179.3(3) . . . . ?
C25 C26 C27 F9 -60.7(4) . . . . ?
C25 C26 C27 F10 57.3(4) . . . . ?
C25 C26 C27 C28 178.1(3) . . . . ?
C25A C26A C27A F9A 57.1(4) . . . . ?
C25A C26A C27A F10A -61.1(4) . . . . ?
C25A C26A C27A C28A 178.7(3) . . . . ?
C26 C27 C28 F11 59.9(4) . . . . ?
C26 C27 C28 F12 -59.4(4) . . . . ?
C26 C27 C28 C29 179.8(3) . . . . ?
C26A C27A C28A F11A -60.4(4) . . . . ?
C26A C27A C28A F12A 59.4(4) . . . . ?
C26A C27A C28A C29A 179.8(3) . . . . ?
C27 C28 C29 F13 174.5(3) . . . . ?
C27 C28 C29 F14 -66.4(4) . . . . ?
C27 C28 C29 F15 54.9(4) . . . . ?
C27A C28A C29A F13A 55.1(4) . . . . ?
C27A C28A C29A F14A -66.8(4) . . . . ?
C27A C28A C29A F15A 174.0(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.835
