# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_ga_lh7
_audit_creation_date             
;
'Wed Dec 04 11:54:00 2013'
;
_audit_update_record             'Wed Dec  4 11:58:12 CET 2013'

_audit_block_code                ga_lh7
_audit_block_refno               1919
_audit_block_usercomment         'LH253, irregular, red'


_shelxl_version_number           2013-4

_vrf_PLAT220_ga_lh7              
;
PROBLEM: Large Non-Solvent    C     Ueq(max)/Ueq(min) ...        4.9 Ratio 
RESPONSE: unresolved disorder in [CF3SO3] Anion
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C52 H32 F14 N8, 4(C F3 O3 S)'
_chemical_formula_sum            'C56 H32 F26 N8 O12 S4'
_chemical_formula_weight         1631.13
_chemical_melting_point          ?
_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_diffrn_ambient_temperature      110(1)
_chemical_oxdiff_formula         'C56 H32 F26 N8 O12 S4'
_chemical_oxdiff_usercomment     'LH253, irregular, red'
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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_symmetry_equiv_pos_as_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                   10.5849(6)
_cell_length_b                   9.8070(4)
_cell_length_c                   29.9716(13)
_cell_angle_alpha                90
_cell_angle_beta                 99.183(5)
_cell_angle_gamma                90
_cell_volume                     3071.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8995
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      69.8990
_cell_measurement_theta_min      4.2470
_shelx_estimated_absorpt_T_max   0.767
_shelx_estimated_absorpt_T_min   0.767
_exptl_absorpt_coefficient_mu    2.795
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.1959
_exptl_crystal_size_mid          0.1290
_exptl_crystal_size_min          0.0934
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            44255
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.847
_diffrn_reflns_theta_min         4.256
_diffrn_detector_area_resol_mean 7.9621
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0162778000
_diffrn_orient_matrix_UB_12      -0.1555287000
_diffrn_orient_matrix_UB_13      0.0034589000
_diffrn_orient_matrix_UB_21      0.0579769000
_diffrn_orient_matrix_UB_22      0.0056638000
_diffrn_orient_matrix_UB_23      0.0505228000
_diffrn_orient_matrix_UB_31      -0.1345207000
_diffrn_orient_matrix_UB_32      0.0212179000
_diffrn_orient_matrix_UB_33      0.0122216000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4499
_reflns_number_total             5881
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         5881
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.028
_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)+(0.0596P)²+6.9083P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1584
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-O11 \\sim S1-O12 \\sim S1-O13
 with sigma of 0.01
 O11-O12 \\sim O11-O13 \\sim O12-O13
 with sigma of 0.01
 C51-F11 \\sim C51-F12 \\sim C51-F13
 with sigma of 0.01
 F11-F12 \\sim F11-F13 \\sim F12-F13
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O11 \\sim O12 \\sim O13 \\sim O21A \\sim O22A \\sim O23A \\sim O21B \\sim O22B
\\sim O23B \\sim S1 \\sim S2A \\sim S2B \\sim C1 \\sim C2 \\sim C3 \\sim C4
\\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C21 \\sim C23
\\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C29 \\sim C30 \\sim C31 \\sim C32
\\sim C33 \\sim C34 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C51 \\sim
C52A \\sim C52B: within 0.5A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Same fragment restrains
{S1, O11, O12, O13, F11, F12, F13, C51}
as
{S2A, O21A, O22A, O23A, F21A, F22A, F23A, C52A}
{S1, O11, O12, O13, F11, F12, F13, C51}
as
{S2B, O21B, O22B, O23B, F21B, F22B, F23B, C52B}
5. Others
 Sof(S2B)=Sof(O21B)=Sof(O22B)=Sof(O23B)=Sof(F21B)=Sof(F22B)=Sof(F23B)=
 Sof(C52B)=1-FVAR(1)
 Sof(S2A)=Sof(O21A)=Sof(O22A)=Sof(O23A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=
 Sof(C52A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C27(H27), C29(H29), C30(H30), C31(H31), C34(H34), C36(H36),
 C37(H37), C38(H38)
6.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C39(H39A,H39B,H39C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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 -0.07018(19) 0.54250(19) 0.45365(7) 0.0353(5) Uani 1 1 d . . . . .
F2 F -0.1345(2) 0.6797(2) 0.39815(7) 0.0407(5) Uani 1 1 d . . . . .
F3 F -0.1704(2) 0.6995(4) 0.51123(8) 0.0658(9) Uani 1 1 d . . . . .
F4 F -0.2016(2) 0.8641(3) 0.46256(13) 0.0762(10) Uani 1 1 d . . . . .
F5 F -0.4113(2) 0.7152(3) 0.47818(10) 0.0612(8) Uani 1 1 d . . . . .
F6 F -0.3778(3) 0.7176(4) 0.41044(11) 0.0894(11) Uani 1 1 d . . . . .
F7 F -0.3334(2) 0.5394(3) 0.45036(10) 0.0585(7) Uani 1 1 d . . . . .
N1 N 0.0839(3) 0.7492(3) 0.49810(8) 0.0235(6) Uani 1 1 d . . . . .
N2 N 0.0767(3) 0.8172(3) 0.42088(9) 0.0254(6) Uani 1 1 d . . . . .
N28 N 0.1940(3) 0.6066(3) 0.65386(9) 0.0266(6) Uani 1 1 d . . . . .
N35 N 0.8457(3) 0.9557(4) 0.72289(10) 0.0444(8) Uani 1 1 d . . . . .
C1 C 0.1969(3) 0.8142(3) 0.50953(10) 0.0206(6) Uani 1 1 d . . . . .
C2 C 0.2584(3) 0.8141(3) 0.55618(10) 0.0212(6) Uani 1 1 d . . . . .
C3 C 0.3763(3) 0.8700(3) 0.56698(10) 0.0215(6) Uani 1 1 d . . . . .
H3 H 0.4177 0.8657 0.5975 0.026 Uiso 1 1 calc R . . . .
C4 C 0.4413(3) 0.9353(3) 0.53441(10) 0.0194(6) Uani 1 1 d . . . . .
C5 C 0.3804(3) 0.9399(3) 0.48855(10) 0.0186(6) Uani 1 1 d . . . . .
C6 C 0.2579(3) 0.8776(3) 0.47657(10) 0.0206(6) Uani 1 1 d . . . . .
C7 C 0.8074(3) 1.1228(3) 0.56831(10) 0.0234(7) Uani 1 1 d . . . . .
C8 C 0.7477(3) 1.0606(3) 0.60331(10) 0.0247(7) Uani 1 1 d . . . . .
C9 C 0.6304(3) 1.0021(3) 0.59143(10) 0.0226(7) Uani 1 1 d . . . . .
H9 H 0.5909 0.9622 0.6146 0.027 Uiso 1 1 calc R . . . .
C10 C 0.5634(3) 0.9974(3) 0.54599(10) 0.0204(6) Uani 1 1 d . . . . .
C21 C 0.0336(3) 0.7550(3) 0.45450(10) 0.0231(7) Uani 1 1 d . . . . .
C23 C -0.0910(3) 0.6751(3) 0.44295(11) 0.0257(7) Uani 1 1 d . . . . .
C24 C -0.1975(4) 0.7280(4) 0.46755(13) 0.0364(9) Uani 1 1 d . . . . .
C25 C -0.3330(4) 0.6733(4) 0.45107(15) 0.0425(10) Uani 1 1 d . . . . .
C26 C 0.1904(3) 0.7525(3) 0.59079(10) 0.0227(7) Uani 1 1 d . . . . .
C27 C 0.2548(3) 0.6660(3) 0.62269(10) 0.0240(7) Uani 1 1 d . . . . .
H27 H 0.3430 0.6479 0.6228 0.029 Uiso 1 1 calc R . . . .
C29 C 0.0695(3) 0.6302(4) 0.65528(11) 0.0318(8) Uani 1 1 d . . . . .
H29 H 0.0288 0.5864 0.6774 0.038 Uiso 1 1 calc R . . . .
C30 C 0.0014(3) 0.7174(4) 0.62471(11) 0.0309(8) Uani 1 1 d . . . . .
H30 H -0.0863 0.7350 0.6258 0.037 Uiso 1 1 calc R . . . .
C31 C 0.0613(3) 0.7797(4) 0.59236(11) 0.0273(7) Uani 1 1 d . . . . .
H31 H 0.0150 0.8408 0.5712 0.033 Uiso 1 1 calc R . . . .
C32 C 0.2667(4) 0.5136(4) 0.68705(13) 0.0405(9) Uani 1 1 d . . . . .
H32A H 0.3304 0.4644 0.6729 0.061 Uiso 1 1 calc GR . . . .
H32B H 0.2080 0.4482 0.6976 0.061 Uiso 1 1 calc GR . . . .
H32C H 0.3100 0.5663 0.7128 0.061 Uiso 1 1 calc GR . . . .
C33 C 0.8100(3) 1.0644(4) 0.65127(11) 0.0299(7) Uani 1 1 d . . . . .
C34 C 0.7951(4) 0.9556(4) 0.67871(11) 0.0357(8) Uani 1 1 d . . . . .
H34 H 0.7480 0.8784 0.6663 0.043 Uiso 1 1 calc R . . . .
C36 C 0.9135(4) 1.0628(5) 0.74215(13) 0.0506(12) Uani 1 1 d . . . . .
H36 H 0.9482 1.0609 0.7734 0.061 Uiso 1 1 calc R . . . .
C37 C 0.9316(5) 1.1729(6) 0.71672(14) 0.0681(17) Uani 1 1 d . . . . .
H37 H 0.9797 1.2484 0.7301 0.082 Uiso 1 1 calc R . . . .
C38 C 0.8803(5) 1.1759(5) 0.67112(13) 0.0561(13) Uani 1 1 d . . . . .
H38 H 0.8929 1.2535 0.6534 0.067 Uiso 1 1 calc R . . . .
C39 C 0.8226(8) 0.8369(6) 0.75122(16) 0.096(2) Uani 1 1 d . . . . .
H39A H 0.7557 0.8598 0.7691 0.144 Uiso 1 1 calc GR . . . .
H39B H 0.9017 0.8138 0.7715 0.144 Uiso 1 1 calc GR . . . .
H39C H 0.7950 0.7587 0.7317 0.144 Uiso 1 1 calc GR . . . .
S1 S 0.66049(8) 0.58331(10) 0.63617(3) 0.0332(2) Uani 1 1 d . . . . .
O11 O 0.7652(3) 0.5539(5) 0.67068(12) 0.0988(17) Uani 1 1 d . . . . .
O12 O 0.5370(2) 0.5466(3) 0.64614(8) 0.0379(6) Uani 1 1 d . . . . .
O13 O 0.6687(3) 0.7140(3) 0.61554(13) 0.0672(10) Uani 1 1 d . . . . .
F11 F 0.8025(3) 0.4794(3) 0.58184(14) 0.0971(14) Uani 1 1 d . . . . .
F12 F 0.6620(4) 0.3447(3) 0.6021(2) 0.175(3) Uani 1 1 d . . . . .
F13 F 0.6038(4) 0.4999(5) 0.55410(11) 0.144(2) Uani 1 1 d . . . . .
C51 C 0.6844(4) 0.4714(4) 0.59102(18) 0.0695(17) Uani 1 1 d . . . . .
S2A S 0.4446(3) -0.0124(4) 0.70398(10) 0.0376(7) Uani 0.605(6) 1 d . . P A 1
O21A O 0.4559(16) -0.1406(13) 0.6827(5) 0.066(4) Uani 0.605(6) 1 d . . P A 1
O22A O 0.4555(16) -0.016(2) 0.7520(4) 0.053(3) Uani 0.605(6) 1 d . . P A 1
O23A O 0.5156(6) 0.0949(8) 0.6863(2) 0.074(2) Uani 0.605(6) 1 d . . P A 1
F21A F 0.2516(7) 0.0462(9) 0.6407(2) 0.048(2) Uani 0.605(6) 1 d . . P A 1
F22A F 0.2005(4) -0.0570(6) 0.69946(15) 0.0657(16) Uani 0.605(6) 1 d . . P A 1
F23A F 0.2591(15) 0.1509(13) 0.7059(5) 0.136(6) Uani 0.605(6) 1 d . . P A 1
C52A C 0.2795(7) 0.0348(8) 0.6854(2) 0.0402(18) Uani 0.605(6) 1 d . . P A 1
S2B S 0.4108(6) -0.0576(6) 0.70915(17) 0.0512(13) Uani 0.395(6) 1 d . . P A 2
O21B O 0.485(3) -0.110(2) 0.6776(8) 0.072(7) Uani 0.395(6) 1 d . . P A 2
O22B O 0.3070(9) -0.1428(9) 0.7157(3) 0.067(3) Uani 0.395(6) 1 d . . P A 2
O23B O 0.482(3) -0.005(4) 0.7503(6) 0.071(8) Uani 0.395(6) 1 d . . P A 2
F21B F 0.4208(13) 0.1801(10) 0.6723(4) 0.114(4) Uani 0.395(6) 1 d . . P A 2
F22B F 0.258(2) 0.056(2) 0.6435(6) 0.133(9) Uani 0.395(6) 1 d . . P A 2
F23B F 0.2514(10) 0.1566(9) 0.7030(4) 0.040(2) Uani 0.395(6) 1 d . . P A 2
C52B C 0.3341(14) 0.0904(12) 0.6818(5) 0.078(5) Uani 0.395(6) 1 d . . 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
F1 C23 1.349(4) . ?
F2 C23 1.349(4) . ?
F3 C24 1.325(5) . ?
F4 C24 1.343(5) . ?
F5 C25 1.316(5) . ?
F6 C25 1.309(5) . ?
F7 C25 1.313(5) . ?
N1 C1 1.350(4) . ?
N1 C21 1.331(4) . ?
N2 C7 1.352(4) 3_676 ?
N2 C21 1.320(4) . ?
N28 C27 1.348(4) . ?
N28 C29 1.345(5) . ?
N28 C32 1.473(4) . ?
N35 C34 1.347(4) . ?
N35 C36 1.348(6) . ?
N35 C39 1.485(6) . ?
C1 C2 1.445(4) . ?
C1 C6 1.409(4) . ?
C2 C3 1.354(4) . ?
C2 C26 1.482(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.432(4) . ?
C4 C5 1.423(4) . ?
C4 C10 1.420(4) . ?
C5 C6 1.426(4) . ?
C5 C10 1.415(4) 3_676 ?
C6 C7 1.411(4) 3_676 ?
C7 N2 1.352(4) 3_676 ?
C7 C6 1.411(4) 3_676 ?
C7 C8 1.444(4) . ?
C8 C9 1.362(5) . ?
C8 C33 1.483(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.432(4) . ?
C10 C5 1.415(4) 3_676 ?
C21 C23 1.525(4) . ?
C23 C24 1.532(5) . ?
C24 C25 1.537(5) . ?
C26 C27 1.375(5) . ?
C26 C31 1.400(5) . ?
C27 H27 0.9500 . ?
C29 H29 0.9500 . ?
C29 C30 1.371(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.383(5) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.371(5) . ?
C33 C38 1.401(5) . ?
C34 H34 0.9500 . ?
C36 H36 0.9500 . ?
C36 C37 1.353(7) . ?
C37 H37 0.9500 . ?
C37 C38 1.388(6) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
S1 O11 1.420(3) . ?
S1 O12 1.433(3) . ?
S1 O13 1.431(3) . ?
S1 C51 1.791(5) . ?
F11 C51 1.324(4) . ?
F12 C51 1.318(5) . ?
F13 C51 1.315(5) . ?
S2A O21A 1.423(9) . ?
S2A O22A 1.427(11) . ?
S2A O23A 1.442(7) . ?
S2A C52A 1.808(7) . ?
F21A C52A 1.329(9) . ?
F22A C52A 1.341(9) . ?
F23A C52A 1.328(10) . ?
S2B O21B 1.420(13) . ?
S2B O22B 1.419(10) . ?
S2B O23B 1.432(15) . ?
S2B C52B 1.796(11) . ?
F21B C52B 1.335(14) . ?
F22B C52B 1.337(15) . ?
F23B C52B 1.330(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
C21 N1 C1 115.4(3) . . ?
C21 N2 C7 115.4(3) . 3_676 ?
C27 N28 C32 118.7(3) . . ?
C29 N28 C27 121.7(3) . . ?
C29 N28 C32 119.6(3) . . ?
C34 N35 C36 121.5(4) . . ?
C34 N35 C39 119.0(4) . . ?
C36 N35 C39 119.4(4) . . ?
N1 C1 C2 119.3(3) . . ?
N1 C1 C6 121.1(3) . . ?
C6 C1 C2 119.5(3) . . ?
C1 C2 C26 118.9(3) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 C26 122.0(3) . . ?
C2 C3 H3 118.6 . . ?
C2 C3 C4 122.9(3) . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 118.6(3) . . ?
C10 C4 C3 122.9(3) . . ?
C10 C4 C5 118.5(3) . . ?
C4 C5 C6 118.9(3) . . ?
C10 C5 C4 122.8(3) 3_676 . ?
C10 C5 C6 118.3(3) 3_676 . ?
C1 C6 C5 120.8(3) . . ?
C1 C6 C7 117.2(3) . 3_676 ?
C7 C6 C5 121.9(3) 3_676 . ?
N2 C7 C6 121.2(3) 3_676 3_676 ?
N2 C7 C8 119.7(3) 3_676 . ?
C6 C7 C8 119.1(3) 3_676 . ?
C7 C8 C33 121.0(3) . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 C33 120.6(3) . . ?
C8 C9 H9 118.2 . . ?
C8 C9 C10 123.7(3) . . ?
C10 C9 H9 118.2 . . ?
C4 C10 C9 122.6(3) . . ?
C5 C10 C4 118.7(3) 3_676 . ?
C5 C10 C9 118.6(3) 3_676 . ?
N1 C21 C23 113.4(3) . . ?
N2 C21 N1 129.5(3) . . ?
N2 C21 C23 117.1(3) . . ?
F1 C23 C21 109.8(3) . . ?
F1 C23 C24 108.5(3) . . ?
F2 C23 F1 106.6(3) . . ?
F2 C23 C21 110.7(3) . . ?
F2 C23 C24 107.9(3) . . ?
C21 C23 C24 113.1(3) . . ?
F3 C24 F4 108.5(3) . . ?
F3 C24 C23 110.1(3) . . ?
F3 C24 C25 106.7(3) . . ?
F4 C24 C23 107.2(3) . . ?
F4 C24 C25 107.4(3) . . ?
C23 C24 C25 116.6(3) . . ?
F5 C25 C24 109.9(3) . . ?
F6 C25 F5 107.5(4) . . ?
F6 C25 F7 108.5(4) . . ?
F6 C25 C24 111.4(4) . . ?
F7 C25 F5 108.7(4) . . ?
F7 C25 C24 110.8(3) . . ?
C27 C26 C2 119.8(3) . . ?
C27 C26 C31 118.2(3) . . ?
C31 C26 C2 122.1(3) . . ?
N28 C27 C26 120.7(3) . . ?
N28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
N28 C29 H29 120.0 . . ?
N28 C29 C30 119.9(3) . . ?
C30 C29 H29 120.0 . . ?
C29 C30 H30 120.2 . . ?
C29 C30 C31 119.6(3) . . ?
C31 C30 H30 120.2 . . ?
C26 C31 H31 120.0 . . ?
C30 C31 C26 119.9(3) . . ?
C30 C31 H31 120.0 . . ?
N28 C32 H32A 109.5 . . ?
N28 C32 H32B 109.5 . . ?
N28 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C8 119.1(3) . . ?
C34 C33 C38 117.2(3) . . ?
C38 C33 C8 123.7(3) . . ?
N35 C34 C33 121.5(4) . . ?
N35 C34 H34 119.2 . . ?
C33 C34 H34 119.2 . . ?
N35 C36 H36 120.2 . . ?
N35 C36 C37 119.6(4) . . ?
C37 C36 H36 120.2 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.2(4) . . ?
C38 C37 H37 119.9 . . ?
C33 C38 H38 120.0 . . ?
C37 C38 C33 120.0(4) . . ?
C37 C38 H38 120.0 . . ?
N35 C39 H39A 109.5 . . ?
N35 C39 H39B 109.5 . . ?
N35 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O11 S1 O12 115.43(18) . . ?
O11 S1 O13 113.7(2) . . ?
O11 S1 C51 103.8(3) . . ?
O12 S1 C51 104.34(17) . . ?
O13 S1 O12 115.81(18) . . ?
O13 S1 C51 101.3(2) . . ?
F11 C51 S1 111.9(3) . . ?
F12 C51 S1 109.5(4) . . ?
F12 C51 F11 108.8(4) . . ?
F13 C51 S1 110.8(3) . . ?
F13 C51 F11 108.7(4) . . ?
F13 C51 F12 107.1(4) . . ?
O21A S2A O22A 115.7(12) . . ?
O21A S2A O23A 113.2(7) . . ?
O21A S2A C52A 103.5(7) . . ?
O22A S2A O23A 115.1(9) . . ?
O22A S2A C52A 103.6(8) . . ?
O23A S2A C52A 103.6(5) . . ?
F21A C52A S2A 112.4(6) . . ?
F21A C52A F22A 108.9(7) . . ?
F22A C52A S2A 110.6(5) . . ?
F23A C52A S2A 107.3(8) . . ?
F23A C52A F21A 111.5(9) . . ?
F23A C52A F22A 106.0(9) . . ?
O21B S2B O23B 115.7(16) . . ?
O21B S2B C52B 104.5(12) . . ?
O22B S2B O21B 113.7(12) . . ?
O22B S2B O23B 113.7(13) . . ?
O22B S2B C52B 103.6(7) . . ?
O23B S2B C52B 103.9(15) . . ?
F21B C52B S2B 110.7(11) . . ?
F21B C52B F22B 108.8(15) . . ?
F22B C52B S2B 110.7(12) . . ?
F23B C52B S2B 117.5(10) . . ?
F23B C52B F21B 108.0(11) . . ?
F23B C52B F22B 100.5(14) . . ?

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 51.9(4) . . . . ?
F1 C23 C24 F4 169.9(3) . . . . ?
F1 C23 C24 C25 -69.8(4) . . . . ?
F2 C23 C24 F3 167.0(3) . . . . ?
F2 C23 C24 F4 -75.0(4) . . . . ?
F2 C23 C24 C25 45.3(4) . . . . ?
F3 C24 C25 F5 49.6(4) . . . . ?
F3 C24 C25 F6 168.5(4) . . . . ?
F3 C24 C25 F7 -70.6(4) . . . . ?
F4 C24 C25 F5 -66.6(5) . . . . ?
F4 C24 C25 F6 52.3(5) . . . . ?
F4 C24 C25 F7 173.2(4) . . . . ?
N1 C1 C2 C3 174.8(3) . . . . ?
N1 C1 C2 C26 -5.0(4) . . . . ?
N1 C1 C6 C5 -176.7(3) . . . . ?
N1 C1 C6 C7 3.6(4) . . . 3_676 ?
N1 C21 C23 F1 -59.9(4) . . . . ?
N1 C21 C23 F2 -177.3(3) . . . . ?
N1 C21 C23 C24 61.4(4) . . . . ?
N2 C7 C8 C9 179.4(3) 3_676 . . . ?
N2 C7 C8 C33 1.6(5) 3_676 . . . ?
N2 C21 C23 F1 119.3(3) . . . . ?
N2 C21 C23 F2 1.9(4) . . . . ?
N2 C21 C23 C24 -119.4(3) . . . . ?
N28 C29 C30 C31 0.6(5) . . . . ?
N35 C36 C37 C38 0.3(8) . . . . ?
C1 N1 C21 N2 -1.5(5) . . . . ?
C1 N1 C21 C23 177.6(3) . . . . ?
C1 C2 C3 C4 2.9(5) . . . . ?
C1 C2 C26 C27 134.2(3) . . . . ?
C1 C2 C26 C31 -45.9(4) . . . . ?
C2 C1 C6 C5 1.0(4) . . . . ?
C2 C1 C6 C7 -178.7(3) . . . 3_676 ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C2 C3 C4 C10 178.1(3) . . . . ?
C2 C26 C27 N28 -178.5(3) . . . . ?
C2 C26 C31 C30 178.6(3) . . . . ?
C3 C2 C26 C27 -45.7(4) . . . . ?
C3 C2 C26 C31 134.2(3) . . . . ?
C3 C4 C5 C6 -0.9(4) . . . . ?
C3 C4 C5 C10 179.7(3) . . . 3_676 ?
C3 C4 C10 C5 -179.6(3) . . . 3_676 ?
C3 C4 C10 C9 -1.3(5) . . . . ?
C4 C5 C6 C1 0.9(4) . . . . ?
C4 C5 C6 C7 -179.4(3) . . . 3_676 ?
C5 C4 C10 C5 -0.5(5) . . . 3_676 ?
C5 C4 C10 C9 177.8(3) . . . . ?
C6 C1 C2 C3 -2.9(4) . . . . ?
C6 C1 C2 C26 177.2(3) . . . . ?
C6 C7 C8 C9 0.8(5) 3_676 . . . ?
C6 C7 C8 C33 -177.1(3) 3_676 . . . ?
C7 N2 C21 N1 4.4(5) 3_676 . . . ?
C7 N2 C21 C23 -174.6(3) 3_676 . . . ?
C7 C8 C9 C10 0.7(5) . . . . ?
C7 C8 C33 C34 -145.8(3) . . . . ?
C7 C8 C33 C38 36.6(6) . . . . ?
C8 C9 C10 C4 179.8(3) . . . . ?
C8 C9 C10 C5 -1.9(5) . . . 3_676 ?
C8 C33 C34 N35 -177.6(3) . . . . ?
C8 C33 C38 C37 177.7(4) . . . . ?
C9 C8 C33 C34 36.4(5) . . . . ?
C9 C8 C33 C38 -141.2(4) . . . . ?
C10 C4 C5 C6 179.9(3) . . . . ?
C10 C4 C5 C10 0.5(5) . . . 3_676 ?
C10 C5 C6 C1 -179.7(3) 3_676 . . . ?
C10 C5 C6 C7 0.0(4) 3_676 . . 3_676 ?
C21 N1 C1 C2 179.6(3) . . . . ?
C21 N1 C1 C6 -2.7(4) . . . . ?
C21 C23 C24 F3 -70.1(4) . . . . ?
C21 C23 C24 F4 47.8(4) . . . . ?
C21 C23 C24 C25 168.2(3) . . . . ?
C23 C24 C25 F5 173.1(3) . . . . ?
C23 C24 C25 F6 -68.0(5) . . . . ?
C23 C24 C25 F7 52.9(5) . . . . ?
C26 C2 C3 C4 -177.2(3) . . . . ?
C27 N28 C29 C30 -0.5(5) . . . . ?
C27 C26 C31 C30 -1.6(5) . . . . ?
C29 N28 C27 C26 -0.6(5) . . . . ?
C29 C30 C31 C26 0.5(5) . . . . ?
C31 C26 C27 N28 1.6(5) . . . . ?
C32 N28 C27 C26 179.4(3) . . . . ?
C32 N28 C29 C30 179.5(3) . . . . ?
C33 C8 C9 C10 178.6(3) . . . . ?
C34 N35 C36 C37 -0.1(7) . . . . ?
C34 C33 C38 C37 0.1(7) . . . . ?
C36 N35 C34 C33 -0.1(6) . . . . ?
C36 C37 C38 C33 -0.3(8) . . . . ?
C38 C33 C34 N35 0.1(6) . . . . ?
C39 N35 C34 C33 177.9(5) . . . . ?
C39 N35 C36 C37 -178.1(5) . . . . ?
O11 S1 C51 F11 -50.1(4) . . . . ?
O11 S1 C51 F12 70.6(4) . . . . ?
O11 S1 C51 F13 -171.5(3) . . . . ?
O12 S1 C51 F11 -171.3(3) . . . . ?
O12 S1 C51 F12 -50.6(4) . . . . ?
O12 S1 C51 F13 67.3(3) . . . . ?
O13 S1 C51 F11 68.0(4) . . . . ?
O13 S1 C51 F12 -171.3(4) . . . . ?
O13 S1 C51 F13 -53.4(3) . . . . ?
O21A S2A C52A F21A -60.4(10) . . . . ?
O21A S2A C52A F22A 61.6(8) . . . . ?
O21A S2A C52A F23A 176.7(10) . . . . ?
O22A S2A C52A F21A 178.5(11) . . . . ?
O22A S2A C52A F22A -59.6(11) . . . . ?
O22A S2A C52A F23A 55.6(13) . . . . ?
O23A S2A C52A F21A 58.0(7) . . . . ?
O23A S2A C52A F22A 179.9(5) . . . . ?
O23A S2A C52A F23A -64.9(9) . . . . ?
O21B S2B C52B F21B -59.2(16) . . . . ?
O21B S2B C52B F22B 61.6(19) . . . . ?
O21B S2B C52B F23B 176.1(15) . . . . ?
O22B S2B C52B F21B -178.5(9) . . . . ?
O22B S2B C52B F22B -57.7(15) . . . . ?
O22B S2B C52B F23B 56.8(12) . . . . ?
O23B S2B C52B F21B 62.4(16) . . . . ?
O23B S2B C52B F22B -176.8(18) . . . . ?
O23B S2B C52B F23B -62.2(17) . . . . ?

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 -6 0 0.0492 -2.0042 -6.0017 -0.0078 0.9660 -0.1506 0.1422
3 5 6 0.0527 3.0033 4.9996 6.0038 -0.8057 0.5058 -0.2245
1 -3 16 0.0566 0.9961 -3.0051 15.9896 0.5065 0.8486 -0.0023
-5 -4 4 0.0634 -5.0070 -4.0010 3.9949 0.7176 -0.1111 0.6375
6 -2 -7 0.0608 6.0061 -2.0008 -7.0029 0.1892 -0.0169 -0.9360
2 6 -1 0.0416 2.0044 6.0019 -0.9918 -0.9695 0.1001 -0.1544
-1 3 -17 0.0766 -0.9958 3.0053 -16.9893 -0.5100 -0.8991 -0.0099
5 -3 -10 0.0641 5.0055 -3.0002 -10.0029 0.3505 -0.2322 -0.8593
6 -2 0 0.0645 6.0046 -2.0024 -0.0054 0.2137 0.3365 -0.8503
-6 2 0 0.0645 -6.0046 2.0024 0.0054 -0.2137 -0.3365 0.8503
-5 -1 14 0.0666 -5.0080 -1.0022 13.9957 0.2858 0.4111 0.8235
-3 -5 -6 0.0568 -3.0033 -4.9996 -6.0038 0.8057 -0.5058 0.2245
-4 5 6 0.0667 -4.0029 5.0016 6.0068 -0.6920 0.0997 0.7180
_cell_oxdiff_length_a            10.5892(6)
_cell_oxdiff_length_b            9.8080(4)
_cell_oxdiff_length_c            29.9583(9)
_cell_oxdiff_angle_alpha         90.051(3)
_cell_oxdiff_angle_beta          99.209(4)
_cell_oxdiff_angle_gamma         90.006(4)
_cell_oxdiff_volume              3071.3(2)
_cell_oxdiff_measurement_reflns_used 8995
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -16.00   17.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega   30.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 35

#__ type_ start__ end____ width___ exp.time_
  3 omega  -27.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega  -58.00  -27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
  5 omega  -69.00    5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   90.0000 74

#__ type_ start__ end____ width___ exp.time_
  6 omega  -17.00   12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
  7 omega  -68.00   17.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
  8 omega   24.00  124.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
  9 omega   82.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 40

#__ type_ start__ end____ width___ exp.time_
 10 omega   25.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 38

#__ type_ start__ end____ width___ exp.time_
 11 omega   24.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 54

#__ type_ start__ end____ width___ exp.time_
 12 omega   24.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 30

#__ type_ start__ end____ width___ exp.time_
 13 omega  -15.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 80

#__ type_ start__ end____ width___ exp.time_
 14 omega   24.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 77

#__ type_ start__ end____ width___ exp.time_
 15 omega   25.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
 16 omega   83.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   79.00  117.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 38

#__ type_ start__ end____ width___ exp.time_
 18 omega   83.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 28

#__ type_ start__ end____ width___ exp.time_
 19 omega  -16.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  -60.0000 95

#__ type_ start__ end____ width___ exp.time_
 20 omega   24.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
 21 omega  -11.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   30.0000 65

#__ type_ start__ end____ width___ exp.time_
 22 omega   63.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 41

#__ type_ start__ end____ width___ exp.time_
 23 omega   24.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 24 omega   24.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 35

#__ type_ start__ end____ width___ exp.time_
 25 omega   24.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 38

#__ type_ start__ end____ width___ exp.time_
 26 omega   24.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 27 omega   24.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 35

#__ type_ start__ end____ width___ exp.time_
 28 omega   60.00  123.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 63

#__ type_ start__ end____ width___ exp.time_
 29 omega   24.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 40

#__ type_ start__ end____ width___ exp.time_
 30 omega   77.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 45

#__ type_ start__ end____ width___ exp.time_
 31 omega   64.00  111.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 47

#__ type_ start__ end____ width___ exp.time_
 32 omega  117.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
 33 omega   78.00  104.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 34 omega   78.00  104.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 35 omega   85.00  132.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
 36 omega   85.00  110.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 37 omega  108.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 69

#__ type_ start__ end____ width___ exp.time_
 38 omega   82.00  145.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 63

#__ type_ start__ end____ width___ exp.time_
 39 omega   78.00  103.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 40 omega   82.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 34

#__ type_ start__ end____ width___ exp.time_
 41 omega   36.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 80

#__ type_ start__ end____ width___ exp.time_
 42 omega   83.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   69.0000  137.4524 26

#__ type_ start__ end____ width___ exp.time_
 43 omega   85.00  175.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 90

#__ type_ start__ end____ width___ exp.time_
 44 omega   85.00  163.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 78

#__ type_ start__ end____ width___ exp.time_
 45 omega  132.00  165.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 33

#__ type_ start__ end____ width___ exp.time_
 46 omega   78.00  103.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 47 omega  115.00  175.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 60

#__ type_ start__ end____ width___ exp.time_
 48 omega   78.00  103.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 49 omega   48.00  137.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -180.0000 89

#__ type_ start__ end____ width___ exp.time_
 50 omega   78.00  103.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 51 omega   86.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 52 omega   82.00  132.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 50

#__ type_ start__ end____ width___ exp.time_
 53 omega   85.00  131.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 46

#__ type_ start__ end____ width___ exp.time_
 54 omega   85.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 55 omega  109.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 65

#__ type_ start__ end____ width___ exp.time_
 56 omega  111.00  168.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 57

#__ type_ start__ end____ width___ exp.time_
 57 omega   78.00  103.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 58 omega   78.00  103.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 59 omega   78.00  104.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 60 omega  123.00  177.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 54

#__ type_ start__ end____ width___ exp.time_
 61 omega   78.00  105.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 62 omega  112.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 66

#__ type_ start__ end____ width___ exp.time_
 63 omega   86.00  115.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   90.0000 29

#__ type_ start__ end____ width___ exp.time_
 64 omega   86.00  175.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 89

#__ type_ start__ end____ width___ exp.time_
 65 omega  128.00  170.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 42

#__ type_ start__ end____ width___ exp.time_
 66 omega   78.00  103.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
 67 omega   82.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 68 omega   85.00  116.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 31

#__ type_ start__ end____ width___ exp.time_
 69 omega   39.00  138.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 99

#__ type_ start__ end____ width___ exp.time_
 70 omega   85.00  111.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 71 omega   36.00  115.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 79

#__ type_ start__ end____ width___ exp.time_
 72 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000 -136.7234 26

#__ type_ start__ end____ width___ exp.time_
 73 omega   87.00  113.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   52.0000    4.5224 26

#__ type_ start__ end____ width___ exp.time_
 74 omega   86.00  112.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   46.0000   67.4578 26

;
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/n'
_symmetry_int_tables_number      14
_chemical_absolute_configuration .
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent EOS'
_diffrn_measurement_specimen_support 'polyimid foil'
_database_code_depnum_ccdc_archive 'CCDC 986570'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ga_lh5
_audit_creation_date             2014-02-12
_audit_update_record             'Wed Feb 12 16:11:49 CET 2014'

_audit_block_code                ga_lh5
_audit_block_refno               1860
_audit_block_usercomment         LH353


_shelxl_version_number           2013-4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C48 H20 F14 N8, 3(C4 H8 O)'
_chemical_formula_sum            'C60 H44 F14 N8 O3'
_chemical_formula_weight         1191.03
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            red
_diffrn_ambient_temperature      100(1)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.096(10)
_cell_length_b                   11.551(5)
_cell_length_c                   22.445(10)
_cell_angle_alpha                90
_cell_angle_beta                 108.873(11)
_cell_angle_gamma                90
_cell_volume                     5176(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8099
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.977
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.7876

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61657
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.659
_diffrn_reflns_theta_min         1.918
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5881
_reflns_number_total             7908
_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       
;
SAINT 8.x (Bruker AXS, 1997-2012). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT 8.x (Bruker AXS, 1997-2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al., 2004)'
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7908
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0554
_refine_ls_restrained_S_all      1.022
_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)+(0.0660P)²+8.4620P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1454
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C51(H51A,
 H51B), C52(H52A,H52B)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.03725(6) -0.05255(9) 0.19307(5) 0.0213(2) Uani 1 1 d . . . . .
F2 F 0.08313(5) 0.11412(9) 0.18640(5) 0.0221(2) Uani 1 1 d . . . . .
F3 F -0.05376(5) -0.01798(11) 0.07482(5) 0.0271(3) Uani 1 1 d . . . . .
F4 F -0.00735(6) 0.14947(10) 0.07048(5) 0.0281(3) Uani 1 1 d . . . . .
F5 F -0.08074(6) 0.05111(10) 0.18046(6) 0.0275(3) Uani 1 1 d . . . . .
F6 F -0.03366(6) 0.21502(10) 0.17898(6) 0.0305(3) Uani 1 1 d . . . . .
F7 F -0.11941(6) 0.16461(14) 0.10148(6) 0.0429(4) Uani 1 1 d . . . . .
N1 N 0.07676(7) -0.14446(12) 0.10212(7) 0.0131(3) Uani 1 1 d . . . . .
N2 N 0.13631(7) 0.03382(11) 0.10386(6) 0.0128(3) Uani 1 1 d . . . . .
N3 N 0.20438(8) 0.36278(12) 0.09290(8) 0.0208(3) Uani 1 1 d . . . . .
N501 N 0.56075(7) -0.08361(14) -0.07034(8) 0.0206(3) Uani 1 1 d . . . . .
C1 C 0.11523(7) -0.19780(13) 0.07262(7) 0.0116(3) Uani 1 1 d . . . . .
C2 C 0.39450(7) -0.18041(13) -0.05776(7) 0.0118(3) Uani 1 1 d . . . . .
C3 C 0.35247(8) -0.12669(13) -0.03110(8) 0.0122(3) Uani 1 1 d . . . . .
H3 H 0.3592(10) -0.0437(18) -0.0232(10) 0.015 Uiso 1 1 d R . . . .
C4 C 0.30062(7) -0.18608(13) -0.01522(7) 0.0110(3) Uani 1 1 d . . . . .
C5 C 0.20901(7) -0.19444(13) 0.02934(7) 0.0106(3) Uani 1 1 d . . . . .
C6 C 0.16690(7) -0.13720(13) 0.05825(7) 0.0109(3) Uani 1 1 d . . . . .
C7 C 0.17507(8) -0.01824(13) 0.07426(7) 0.0113(3) Uani 1 1 d . . . . .
C8 C 0.22747(8) 0.04694(13) 0.06069(7) 0.0118(3) Uani 1 1 d . . . . .
C9 C 0.26686(8) -0.00933(13) 0.03179(8) 0.0121(3) Uani 1 1 d . . . . .
H9 H 0.3007(10) 0.0332(18) 0.0221(10) 0.015 Uiso 1 1 d R . . . .
C10 C 0.25943(7) -0.12959(13) 0.01486(7) 0.0109(3) Uani 1 1 d . . . . .
C21 C 0.09128(8) -0.03393(13) 0.11633(8) 0.0128(3) Uani 1 1 d . . . . .
C23 C 0.04976(8) 0.02353(13) 0.15255(8) 0.0132(3) Uani 1 1 d . . . . .
C24 C -0.01828(8) 0.06974(14) 0.10995(8) 0.0159(3) Uani 1 1 d . . . . .
C25 C -0.06363(8) 0.12648(15) 0.14391(8) 0.0183(3) Uani 1 1 d . . . . .
C26 C 0.44650(8) -0.11095(13) -0.07287(8) 0.0128(3) Uani 1 1 d . . . . .
C27 C 0.51275(8) -0.14768(15) -0.05918(8) 0.0168(3) Uani 1 1 d . . . . .
H27 H 0.5245 -0.2221 -0.0410 0.020 Uiso 1 1 calc R . . . .
C28 C 0.54297(9) 0.02033(16) -0.09711(9) 0.0198(3) Uani 1 1 d . . . . .
H28 H 0.5762 0.0658 -0.1062 0.024 Uiso 1 1 calc R . . . .
C29 C 0.47893(9) 0.06495(15) -0.11221(9) 0.0206(3) Uani 1 1 d . . . . .
H29 H 0.4686 0.1393 -0.1309 0.025 Uiso 1 1 calc R . . . .
C30 C 0.42993(8) -0.00135(14) -0.09945(8) 0.0169(3) Uani 1 1 d . . . . .
H30 H 0.3856 0.0276 -0.1087 0.020 Uiso 1 1 calc R . . . .
C31 C 0.24163(8) 0.17008(13) 0.07913(8) 0.0130(3) Uani 1 1 d . . . . .
C32 C 0.19177(9) 0.25192(14) 0.07587(8) 0.0169(3) Uani 1 1 d . . . . .
H32 H 0.1464 0.2274 0.0607 0.020 Uiso 1 1 calc R . . . .
C33 C 0.26836(10) 0.39700(15) 0.11386(9) 0.0212(4) Uani 1 1 d . . . . .
H33 H 0.2778 0.4750 0.1272 0.025 Uiso 1 1 calc R . . . .
C34 C 0.32123(9) 0.32436(15) 0.11706(9) 0.0212(4) Uani 1 1 d . . . . .
H34 H 0.3660 0.3525 0.1309 0.025 Uiso 1 1 calc R . . . .
C35 C 0.30782(8) 0.20943(14) 0.09967(9) 0.0176(3) Uani 1 1 d . . . . .
H35 H 0.3435 0.1577 0.1017 0.021 Uiso 1 1 calc R . . . .
O41 O 0.21106(7) -0.12654(12) 0.22075(7) 0.0276(3) Uani 1 1 d . . . . .
C41 C 0.21824(11) -0.24860(18) 0.23169(10) 0.0291(4) Uani 1 1 d . . . . .
H41A H 0.1756 -0.2891 0.2103 0.035 Uiso 1 1 calc R . . . .
H41B H 0.2319 -0.2657 0.2773 0.035 Uiso 1 1 calc R . . . .
C42 C 0.27248(11) -0.28610(18) 0.20444(11) 0.0300(4) Uani 1 1 d . . . . .
H42A H 0.2525 -0.3127 0.1604 0.036 Uiso 1 1 calc R . . . .
H42B H 0.3000 -0.3493 0.2297 0.036 Uiso 1 1 calc R . . . .
C43 C 0.31469(12) -0.1765(2) 0.20774(13) 0.0389(5) Uani 1 1 d . . . . .
H43A H 0.3609 -0.1875 0.2368 0.047 Uiso 1 1 calc R . . . .
H43B H 0.3166 -0.1554 0.1656 0.047 Uiso 1 1 calc R . . . .
C44 C 0.27763(10) -0.08378(18) 0.23261(10) 0.0283(4) Uani 1 1 d . . . . .
H44A H 0.2999 -0.0714 0.2783 0.034 Uiso 1 1 calc R . . . .
H44B H 0.2769 -0.0094 0.2105 0.034 Uiso 1 1 calc R . . . .
O51 O 0.5000 -0.0003(2) -0.2500 0.0383(5) Uani 1 2 d S T P B .
C51 C 0.44200(13) -0.0724(2) -0.26110(11) 0.0380(5) Uani 1 1 d . . . . .
H51A H 0.4071 -0.0501 -0.3009 0.046 Uiso 1 1 calc R . . A .
H51B H 0.4232 -0.0647 -0.2262 0.046 Uiso 1 1 calc R . . A .
C52 C 0.46494(16) -0.1953(3) -0.2651(2) 0.0747(11) Uani 1 1 d . . . B 2
H52A H 0.4428 -0.2491 -0.2437 0.090 Uiso 1 1 calc R . . B 2
H52B H 0.4540 -0.2194 -0.3097 0.090 Uiso 1 1 calc R . . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C23 1.3507(19) . ?
F2 C23 1.3498(18) . ?
F3 C24 1.352(2) . ?
F4 C24 1.348(2) . ?
F5 C25 1.324(2) . ?
F6 C25 1.320(2) . ?
F7 C25 1.327(2) . ?
N1 C1 1.3507(19) . ?
N1 C21 1.328(2) . ?
N2 C7 1.350(2) . ?
N2 C21 1.329(2) . ?
N3 C32 1.338(2) . ?
N3 C33 1.337(2) . ?
N501 C27 1.342(2) . ?
N501 C28 1.341(2) . ?
C1 C2 1.445(2) 7_545 ?
C1 C6 1.418(2) . ?
C2 C1 1.445(2) 7_545 ?
C2 C3 1.369(2) . ?
C2 C26 1.484(2) . ?
C3 H3 0.98(2) . ?
C3 C4 1.431(2) . ?
C4 C5 1.416(2) 7_545 ?
C4 C10 1.420(2) . ?
C5 C4 1.416(2) 7_545 ?
C5 C6 1.421(2) . ?
C5 C10 1.422(2) . ?
C6 C7 1.417(2) . ?
C7 C8 1.449(2) . ?
C8 C9 1.372(2) . ?
C8 C31 1.485(2) . ?
C9 H9 0.95(2) . ?
C9 C10 1.435(2) . ?
C21 C23 1.526(2) . ?
C23 C24 1.540(2) . ?
C24 C25 1.548(2) . ?
C26 C27 1.396(2) . ?
C26 C30 1.395(2) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C28 C29 1.382(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.389(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.399(2) . ?
C31 C35 1.397(2) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C33 C34 1.379(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.387(2) . ?
C35 H35 0.9500 . ?
O41 C41 1.431(2) . ?
O41 C44 1.430(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.524(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.536(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.534(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
O51 C51 1.434(3) . ?
O51 C51 1.434(3) 2_654 ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.512(4) . ?
C52 C52 1.414(7) 2_654 ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 N1 C1 115.33(13) . . ?
C21 N2 C7 115.43(14) . . ?
C33 N3 C32 117.91(15) . . ?
C28 N501 C27 117.32(15) . . ?
N1 C1 C2 119.62(14) . 7_545 ?
N1 C1 C6 120.96(14) . . ?
C6 C1 C2 119.37(13) . 7_545 ?
C1 C2 C26 122.26(13) 7_545 . ?
C3 C2 C1 118.60(14) . 7_545 ?
C3 C2 C26 119.08(14) . . ?
C2 C3 H3 116.6(12) . . ?
C2 C3 C4 123.18(14) . . ?
C4 C3 H3 120.3(12) . . ?
C5 C4 C3 118.52(13) 7_545 . ?
C5 C4 C10 119.27(13) 7_545 . ?
C10 C4 C3 122.20(14) . . ?
C4 C5 C6 119.35(13) 7_545 . ?
C4 C5 C10 121.74(13) 7_545 . ?
C6 C5 C10 118.91(13) . . ?
C1 C6 C5 120.95(14) . . ?
C7 C6 C1 117.43(13) . . ?
C7 C6 C5 121.62(13) . . ?
N2 C7 C6 120.89(14) . . ?
N2 C7 C8 119.78(14) . . ?
C6 C7 C8 119.29(13) . . ?
C7 C8 C31 122.52(13) . . ?
C9 C8 C7 118.24(14) . . ?
C9 C8 C31 119.20(14) . . ?
C8 C9 H9 118.7(12) . . ?
C8 C9 C10 123.55(14) . . ?
C10 C9 H9 117.8(12) . . ?
C4 C10 C5 118.99(13) . . ?
C4 C10 C9 122.64(13) . . ?
C5 C10 C9 118.36(13) . . ?
N1 C21 N2 129.87(14) . . ?
N1 C21 C23 114.74(13) . . ?
N2 C21 C23 115.39(14) . . ?
F1 C23 C21 110.27(13) . . ?
F1 C23 C24 107.32(13) . . ?
F2 C23 F1 107.78(13) . . ?
F2 C23 C21 110.62(13) . . ?
F2 C23 C24 107.00(13) . . ?
C21 C23 C24 113.60(14) . . ?
F3 C24 C23 109.36(13) . . ?
F3 C24 C25 106.90(14) . . ?
F4 C24 F3 107.98(14) . . ?
F4 C24 C23 108.76(13) . . ?
F4 C24 C25 107.36(14) . . ?
C23 C24 C25 116.20(14) . . ?
F5 C25 F7 107.86(15) . . ?
F5 C25 C24 111.25(14) . . ?
F6 C25 F5 108.29(15) . . ?
F6 C25 F7 108.25(15) . . ?
F6 C25 C24 111.61(14) . . ?
F7 C25 C24 109.45(15) . . ?
C27 C26 C2 123.13(15) . . ?
C30 C26 C2 119.14(14) . . ?
C30 C26 C27 117.67(14) . . ?
N501 C27 C26 123.61(16) . . ?
N501 C27 H27 118.2 . . ?
C26 C27 H27 118.2 . . ?
N501 C28 H28 118.2 . . ?
N501 C28 C29 123.61(15) . . ?
C29 C28 H28 118.2 . . ?
C28 C29 H29 120.7 . . ?
C28 C29 C30 118.53(17) . . ?
C30 C29 H29 120.7 . . ?
C26 C30 H30 120.4 . . ?
C29 C30 C26 119.24(16) . . ?
C29 C30 H30 120.4 . . ?
C32 C31 C8 123.57(15) . . ?
C35 C31 C8 119.55(14) . . ?
C35 C31 C32 116.86(15) . . ?
N3 C32 C31 123.72(16) . . ?
N3 C32 H32 118.1 . . ?
C31 C32 H32 118.1 . . ?
N3 C33 H33 118.5 . . ?
N3 C33 C34 123.07(16) . . ?
C34 C33 H33 118.5 . . ?
C33 C34 H34 120.7 . . ?
C33 C34 C35 118.68(17) . . ?
C35 C34 H34 120.7 . . ?
C31 C35 H35 120.2 . . ?
C34 C35 C31 119.70(15) . . ?
C34 C35 H35 120.2 . . ?
C44 O41 C41 105.38(15) . . ?
O41 C41 H41A 110.7 . . ?
O41 C41 H41B 110.7 . . ?
O41 C41 C42 105.23(17) . . ?
H41A C41 H41B 108.8 . . ?
C42 C41 H41A 110.7 . . ?
C42 C41 H41B 110.7 . . ?
C41 C42 H42A 110.9 . . ?
C41 C42 H42B 110.9 . . ?
C41 C42 C43 104.20(17) . . ?
H42A C42 H42B 108.9 . . ?
C43 C42 H42A 110.9 . . ?
C43 C42 H42B 110.9 . . ?
C42 C43 H43A 111.0 . . ?
C42 C43 H43B 111.0 . . ?
H43A C43 H43B 109.0 . . ?
C44 C43 C42 103.73(18) . . ?
C44 C43 H43A 111.0 . . ?
C44 C43 H43B 111.0 . . ?
O41 C44 C43 106.06(17) . . ?
O41 C44 H44A 110.5 . . ?
O41 C44 H44B 110.5 . . ?
C43 C44 H44A 110.5 . . ?
C43 C44 H44B 110.5 . . ?
H44A C44 H44B 108.7 . . ?
C51 O51 C51 109.0(3) 2_654 . ?
O51 C51 H51A 110.4 . . ?
O51 C51 H51B 110.4 . . ?
O51 C51 C52 106.5(2) . . ?
H51A C51 H51B 108.6 . . ?
C52 C51 H51A 110.4 . . ?
C52 C51 H51B 110.4 . . ?
C51 C52 H52A 110.5 . . ?
C51 C52 H52B 110.5 . . ?
C52 C52 C51 106.1(2) 2_654 . ?
C52 C52 H52A 110.5 2_654 . ?
C52 C52 H52B 110.5 2_654 . ?
H52A C52 H52B 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
F1 C23 C24 F3 -64.66(16) . . . . ?
F1 C23 C24 F4 177.64(12) . . . . ?
F1 C23 C24 C25 56.42(18) . . . . ?
F2 C23 C24 F3 179.88(12) . . . . ?
F2 C23 C24 F4 62.18(16) . . . . ?
F2 C23 C24 C25 -59.04(17) . . . . ?
F3 C24 C25 F5 59.90(18) . . . . ?
F3 C24 C25 F6 -179.02(14) . . . . ?
F3 C24 C25 F7 -59.20(19) . . . . ?
F4 C24 C25 F5 175.56(14) . . . . ?
F4 C24 C25 F6 -63.36(19) . . . . ?
F4 C24 C25 F7 56.46(19) . . . . ?
N1 C1 C6 C5 177.62(15) . . . . ?
N1 C1 C6 C7 -1.9(2) . . . . ?
N1 C21 C23 F1 36.01(19) . . . . ?
N1 C21 C23 F2 155.14(14) . . . . ?
N1 C21 C23 C24 -84.50(18) . . . . ?
N2 C7 C8 C9 178.60(15) . . . . ?
N2 C7 C8 C31 1.1(2) . . . . ?
N2 C21 C23 F1 -143.96(15) . . . . ?
N2 C21 C23 F2 -24.8(2) . . . . ?
N2 C21 C23 C24 95.53(17) . . . . ?
N3 C33 C34 C35 -2.1(3) . . . . ?
N501 C28 C29 C30 -0.4(3) . . . . ?
C1 N1 C21 N2 2.9(3) . . . . ?
C1 N1 C21 C23 -177.08(14) . . . . ?
C1 C2 C3 C4 2.2(2) 7_545 . . . ?
C1 C2 C26 C27 -47.4(2) 7_545 . . . ?
C1 C2 C26 C30 135.59(17) 7_545 . . . ?
C1 C6 C7 N2 2.0(2) . . . . ?
C1 C6 C7 C8 179.71(14) . . . . ?
C2 C1 C6 C5 0.2(2) 7_545 . . . ?
C2 C1 C6 C7 -179.34(14) 7_545 . . . ?
C2 C3 C4 C5 -1.8(2) . . . 7_545 ?
C2 C3 C4 C10 177.27(16) . . . . ?
C2 C26 C27 N501 -177.24(16) . . . . ?
C2 C26 C30 C29 178.44(15) . . . . ?
C3 C2 C26 C27 135.26(17) . . . . ?
C3 C2 C26 C30 -41.8(2) . . . . ?
C3 C4 C10 C5 -179.82(15) . . . . ?
C3 C4 C10 C9 -0.3(2) . . . . ?
C4 C5 C6 C1 -0.5(2) 7_545 . . . ?
C4 C5 C6 C7 179.00(15) 7_545 . . . ?
C4 C5 C10 C4 0.7(3) 7_545 . . . ?
C4 C5 C10 C9 -178.81(15) 7_545 . . . ?
C5 C4 C10 C5 -0.7(2) 7_545 . . . ?
C5 C4 C10 C9 178.81(15) 7_545 . . . ?
C5 C6 C7 N2 -177.47(15) . . . . ?
C5 C6 C7 C8 0.2(2) . . . . ?
C6 C5 C10 C4 -178.69(14) . . . . ?
C6 C5 C10 C9 1.8(2) . . . . ?
C6 C7 C8 C9 0.9(2) . . . . ?
C6 C7 C8 C31 -176.58(15) . . . . ?
C7 N2 C21 N1 -2.7(3) . . . . ?
C7 N2 C21 C23 177.22(14) . . . . ?
C7 C8 C9 C10 -0.7(2) . . . . ?
C7 C8 C31 C32 -38.8(2) . . . . ?
C7 C8 C31 C35 142.70(17) . . . . ?
C8 C9 C10 C4 179.79(15) . . . . ?
C8 C9 C10 C5 -0.7(2) . . . . ?
C8 C31 C32 N3 179.48(16) . . . . ?
C8 C31 C35 C34 -179.87(16) . . . . ?
C9 C8 C31 C32 143.69(17) . . . . ?
C9 C8 C31 C35 -34.8(2) . . . . ?
C10 C5 C6 C1 178.95(15) . . . . ?
C10 C5 C6 C7 -1.5(2) . . . . ?
C21 N1 C1 C2 177.13(15) . . . 7_545 ?
C21 N1 C1 C6 -0.3(2) . . . . ?
C21 N2 C7 C6 0.0(2) . . . . ?
C21 N2 C7 C8 -177.63(14) . . . . ?
C21 C23 C24 F3 57.50(17) . . . . ?
C21 C23 C24 F4 -60.20(17) . . . . ?
C21 C23 C24 C25 178.58(14) . . . . ?
C23 C24 C25 F5 -62.48(19) . . . . ?
C23 C24 C25 F6 58.6(2) . . . . ?
C23 C24 C25 F7 178.42(15) . . . . ?
C26 C2 C3 C4 179.61(15) . . . . ?
C27 N501 C28 C29 1.5(3) . . . . ?
C27 C26 C30 C29 1.3(2) . . . . ?
C28 N501 C27 C26 -1.2(3) . . . . ?
C28 C29 C30 C26 -1.0(3) . . . . ?
C30 C26 C27 N501 -0.2(3) . . . . ?
C31 C8 C9 C10 176.90(15) . . . . ?
C32 N3 C33 C34 1.7(3) . . . . ?
C32 C31 C35 C34 1.6(3) . . . . ?
C33 N3 C32 C31 0.4(3) . . . . ?
C33 C34 C35 C31 0.3(3) . . . . ?
C35 C31 C32 N3 -2.0(3) . . . . ?
O41 C41 C42 C43 26.0(2) . . . . ?
C41 O41 C44 C43 37.3(2) . . . . ?
C41 C42 C43 C44 -3.7(2) . . . . ?
C42 C43 C44 O41 -19.8(2) . . . . ?
C44 O41 C41 C42 -39.7(2) . . . . ?
O51 C51 C52 C52 20.4(5) . . . 2_654 ?
C51 O51 C51 C52 -7.4(2) 2_654 . . . ?

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'C 2/c'
_symmetry_int_tables_number      15

_chemical_absolute_configuration .

_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            CCD-PXL-KAF2



_database_code_depnum_ccdc_archive 'CCDC 986571'
