# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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 
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data_L-TBACl_H2O
_database_code_depnum_ccdc_archive 'CCDC 1551283'
_audit_update_record             
;
2017-05-20 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H14 F12 N4 O2, C16 H36 N, Cl, O'
_chemical_formula_sum            'C40 H50 Cl F12 N5 O3'
_chemical_formula_weight         912.30
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           ?
_space_group_name_H-M_alt        'I 2/c'
_space_group_name_Hall           '-I 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   25.9705(11)
_cell_length_b                   8.7538(5)
_cell_length_c                   45.267(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.053(5)
_cell_angle_gamma                90
_cell_volume                     9983.0(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4602
_cell_measurement_theta_min      3.5330
_cell_measurement_theta_max      22.660

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             3792.0
_exptl_transmission_factor_min   0.955
_exptl_transmission_factor_max   0.972
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.159
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22919
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         2.964
_diffrn_reflns_theta_max         28.867
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12349
_reflns_number_gt                4724
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1250P)²+0.0010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         12349
_refine_ls_number_parameters     654
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0969
_refine_ls_wR_factor_ref         0.3049
_refine_ls_wR_factor_gt          0.2723
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_restrained_S_all      1.186
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002

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
F2A F 0.3024(6) 0.610(2) 0.6475(3) 0.183(7) Uani 0.5 1 d . . P A 1
F3A F 0.3105(6) 0.808(2) 0.6221(5) 0.160(8) Uani 0.5 1 d . . P A 1
F5A F 0.4487(6) 0.4690(11) 0.53869(19) 0.138(4) Uani 0.5 1 d . . P B 1
F6A F 0.4491(5) 0.7023(10) 0.5470(3) 0.162(6) Uani 0.5 1 d . . P B 1
F7A F 0.7074(12) -0.030(2) 0.5317(3) 0.192(7) Uani 0.5 1 d . . P C 1
F8A F 0.6822(10) 0.1669(19) 0.5141(6) 0.222(9) Uani 0.5 1 d . . P C 1
F9A F 0.7433(9) 0.069(4) 0.5012(5) 0.221(9) Uani 0.5 1 d . . P C 1
F11A F 0.9005(6) 0.3638(18) 0.5364(3) 0.177(6) Uani 0.5 1 d . . P D 1
F12A F 0.9255(7) 0.390(2) 0.5791(4) 0.199(9) Uani 0.5 1 d . . P D 1
F2B F 0.2866(4) 0.5828(11) 0.6307(3) 0.128(4) Uani 0.5 1 d . . P A 2
F3B F 0.3266(6) 0.788(2) 0.6351(5) 0.150(6) Uani 0.5 1 d . . P A 2
F5B F 0.4124(6) 0.4586(17) 0.5293(3) 0.191(6) Uani 0.5 1 d . . P B 2
F6B F 0.4702(4) 0.635(3) 0.5471(2) 0.232(10) Uani 0.5 1 d . . P B 2
F7B F 0.7447(6) -0.0437(15) 0.5206(4) 0.146(4) Uani 0.5 1 d . . P C 2
F8B F 0.6769(5) 0.068(4) 0.5291(4) 0.197(11) Uani 0.5 1 d . . P C 2
F9B F 0.7161(6) 0.1552(19) 0.4971(2) 0.131(4) Uani 0.5 1 d . . P C 2
F11B F 0.8856(5) 0.420(2) 0.5322(3) 0.196(9) Uani 0.5 1 d . . P D 2
F12B F 0.9324(5) 0.3484(13) 0.5790(5) 0.138(6) Uani 0.5 1 d . . P D 2
Cl1 Cl 0.36247(7) 0.1978(3) 0.69058(4) 0.1850(9) Uani 1 1 d . . . . .
O2 O 0.68828(9) 0.2182(4) 0.61993(5) 0.0981(9) Uani 1 1 d . . . . .
O1 O 0.55225(9) 0.3881(3) 0.63366(6) 0.0952(8) Uani 1 1 d . . . . .
N3 N 0.73732(10) 0.2361(3) 0.66886(6) 0.0757(8) Uani 1 1 d . . . . .
H3N H 0.7694 0.2451 0.6796 0.091 Uiso 1 1 calc R U . . .
N4 N 0.77621(10) 0.2756(4) 0.62937(6) 0.0791(8) Uani 1 1 d . . . . .
H4N H 0.8028 0.3061 0.6435 0.095 Uiso 1 1 calc R U . . .
N2 N 0.55549(10) 0.2879(3) 0.68026(6) 0.0744(8) Uani 1 1 d . . . . .
H2N H 0.5357 0.2660 0.6924 0.089 Uiso 1 1 calc R U . . .
N5 N 0.40147(11) 0.1756(3) 0.38338(7) 0.0809(9) Uani 1 1 d . . . . .
F1 F 0.27222(16) 0.6690(9) 0.59677(15) 0.248(3) Uani 1 1 d . . . . .
F10 F 0.88518(17) 0.5508(4) 0.56506(15) 0.197(2) Uani 1 1 d . . . . .
C14 C 0.69777(12) 0.2185(4) 0.68485(7) 0.0623(8) Uani 1 1 d . . . . .
C16 C 0.73011(13) 0.2406(4) 0.63802(8) 0.0734(9) Uani 1 1 d . . . . .
N1 N 0.47843(10) 0.3877(3) 0.65202(6) 0.0786(8) Uani 1 1 d . . . . .
H1N H 0.4662 0.3572 0.6671 0.094 Uiso 1 1 calc R U . . .
C10 C 0.60890(11) 0.2474(4) 0.69032(7) 0.0627(8) Uani 1 1 d . . . . .
C15 C 0.64554(11) 0.2606(4) 0.67276(7) 0.0629(8) Uani 1 1 d . . . . .
H15 H 0.6351 0.2975 0.6529 0.075 Uiso 1 1 calc R U . . .
C9 C 0.53075(12) 0.3573(4) 0.65375(8) 0.0667(8) Uani 1 1 d . . . . .
F4 F 0.38562(17) 0.6374(7) 0.52752(8) 0.1863(17) Uani 1 1 d . . . . .
C17 C 0.78374(12) 0.2662(4) 0.59999(7) 0.0659(8) Uani 1 1 d . . . . .
C24 C 0.82859(12) 0.3345(4) 0.59431(8) 0.0698(9) Uani 1 1 d . . . . .
H24 H 0.8516 0.3873 0.6099 0.084 Uiso 1 1 calc R U . . .
C7 C 0.44272(12) 0.4629(4) 0.62849(8) 0.0704(9) Uani 1 1 d . . . . .
C22 C 0.83952(13) 0.3259(4) 0.56672(9) 0.0725(9) Uani 1 1 d . . . . .
C4 C 0.41384(13) 0.5582(4) 0.57757(9) 0.0757(9) Uani 1 1 d . . . . .
C6 C 0.45139(12) 0.4824(4) 0.59979(8) 0.0723(9) Uani 1 1 d . . . . .
H6 H 0.4822 0.4449 0.5954 0.087 Uiso 1 1 calc R U . . .
C8 C 0.39639(12) 0.5197(4) 0.63470(9) 0.0799(10) Uani 1 1 d . . . . .
H8 H 0.3903 0.5061 0.6539 0.096 Uiso 1 1 calc R U . . .
C13 C 0.71308(13) 0.1625(4) 0.71410(8) 0.0794(10) Uani 1 1 d . . . . .
H13 H 0.7480 0.1320 0.7221 0.095 Uiso 1 1 calc R U . . .
C11 C 0.62480(14) 0.1900(5) 0.71996(8) 0.0832(11) Uani 1 1 d . . . . .
H11 H 0.6003 0.1781 0.7317 0.100 Uiso 1 1 calc R U . . .
C19 C 0.76062(14) 0.1797(4) 0.54846(8) 0.0766(9) Uani 1 1 d . . . . .
C29 C 0.39603(15) 0.3115(4) 0.40368(10) 0.0877(11) Uani 1 1 d . . . . .
H29A H 0.4275 0.3149 0.4204 0.105 Uiso 1 1 calc R U . . .
H29B H 0.3957 0.4042 0.3919 0.105 Uiso 1 1 calc R U . . .
C18 C 0.75009(13) 0.1880(4) 0.57662(8) 0.0760(10) Uani 1 1 d . . . . .
H18 H 0.7200 0.1406 0.5800 0.091 Uiso 1 1 calc R U . . .
C2 C 0.35961(13) 0.5956(4) 0.61258(11) 0.0837(11) Uani 1 1 d . . . . .
C21 C 0.80517(16) 0.2480(4) 0.54270(9) 0.0821(10) Uani 1 1 d . . . . .
H21 H 0.8122 0.2425 0.5235 0.098 Uiso 1 1 calc R U . . .
C3 C 0.36782(14) 0.6155(4) 0.58365(11) 0.0877(12) Uani 1 1 d . . . . .
H3 H 0.3429 0.6663 0.5686 0.105 Uiso 1 1 calc R U . . .
C12 C 0.67649(15) 0.1519(5) 0.73132(9) 0.0951(12) Uani 1 1 d . . . . .
H12 H 0.6874 0.1177 0.7513 0.114 Uiso 1 1 calc R U . . .
C1 C 0.31297(17) 0.6655(7) 0.62022(15) 0.1078(15) Uani 1 1 d . . . . .
C5 C 0.42531(19) 0.5777(6) 0.54712(11) 0.0999(14) Uani 1 1 d . . . . .
C23 C 0.8866(2) 0.4037(5) 0.56068(15) 0.0972(13) Uani 1 1 d . . . . .
C20 C 0.7244(2) 0.0923(8) 0.52407(12) 0.1084(15) Uani 1 1 d . . . . .
C28 C 0.4711(3) -0.1807(10) 0.4755(2) 0.210(4) Uani 1 1 d . . . . .
H28A H 0.5071 -0.1475 0.4781 0.315 Uiso 1 1 calc R U . . .
H28B H 0.4706 -0.2878 0.4800 0.315 Uiso 1 1 calc R U . . .
H28C H 0.4550 -0.1246 0.4891 0.315 Uiso 1 1 calc R U . . .
C33 C 0.35372(16) 0.1648(5) 0.35647(10) 0.0957(12) Uani 1 1 d . . . . .
H33A H 0.3585 0.0769 0.3443 0.115 Uiso 1 1 calc R U . . .
H33B H 0.3226 0.1456 0.3642 0.115 Uiso 1 1 calc R U . . .
C25 C 0.40290(15) 0.0244(5) 0.40107(10) 0.0929(12) Uani 1 1 d . . . . .
H25A H 0.3682 0.0092 0.4051 0.111 Uiso 1 1 calc R U . . .
H25B H 0.4084 -0.0582 0.3879 0.111 Uiso 1 1 calc R U . . .
C37 C 0.45254(16) 0.1996(5) 0.37402(11) 0.0972(12) Uani 1 1 d . . . . .
H37A H 0.4809 0.2116 0.3923 0.117 Uiso 1 1 calc R U . . .
H37B H 0.4499 0.2947 0.3627 0.117 Uiso 1 1 calc R U . . .
C26 C 0.44343(17) 0.0100(6) 0.43043(11) 0.1102(14) Uani 1 1 d . . . . .
H26A H 0.4367 0.0841 0.4450 0.132 Uiso 1 1 calc R U . . .
H26B H 0.4786 0.0286 0.4274 0.132 Uiso 1 1 calc R U . . .
C34 C 0.3428(2) 0.3003(6) 0.33608(12) 0.1204(16) Uani 1 1 d . . . . .
H34A H 0.3749 0.3279 0.3300 0.145 Uiso 1 1 calc R U . . .
H34B H 0.3330 0.3858 0.3472 0.145 Uiso 1 1 calc R U . . .
C31 C 0.3522(3) 0.4410(7) 0.43975(16) 0.150(2) Uani 1 1 d . . . . .
H31A H 0.3862 0.4343 0.4544 0.180 Uiso 1 1 calc R U . . .
H31B H 0.3510 0.5381 0.4293 0.180 Uiso 1 1 calc R U . . .
C38 C 0.4682(2) 0.0749(7) 0.35488(14) 0.141(2) Uani 1 1 d . . . . .
H38A H 0.4442 0.0712 0.3348 0.169 Uiso 1 1 calc R U . E 1
H38B H 0.4686 -0.0241 0.3646 0.169 Uiso 1 1 calc R U . E 1
C32 C 0.3097(3) 0.4392(9) 0.45642(17) 0.181(3) Uani 1 1 d . . . . .
H32A H 0.2770 0.4730 0.4431 0.271 Uiso 1 1 calc R U . . .
H32B H 0.3191 0.5062 0.4737 0.271 Uiso 1 1 calc R U . . .
H32C H 0.3054 0.3372 0.4632 0.271 Uiso 1 1 calc R U . . .
C30 C 0.34861(19) 0.3137(6) 0.41672(13) 0.1149(15) Uani 1 1 d . . . . .
H30A H 0.3457 0.2164 0.4265 0.138 Uiso 1 1 calc R U . . .
H30B H 0.3169 0.3273 0.4004 0.138 Uiso 1 1 calc R U . . .
C39A C 0.5275(5) 0.1246(16) 0.3529(2) 0.098(4) Uani 0.5 1 d . . P F 1
H39A H 0.5257 0.2198 0.3418 0.117 Uiso 0.5 1 calc R U P F 1
H39B H 0.5494 0.1412 0.3733 0.117 Uiso 0.5 1 calc R U P F 1
C39B C 0.5088(6) 0.136(2) 0.3351(5) 0.202(10) Uani 0.5 1 d . . P F 2
H39C H 0.4912 0.1432 0.3136 0.242 Uiso 0.5 1 calc R U P F 2
H39D H 0.5235 0.2346 0.3423 0.242 Uiso 0.5 1 calc R U P F 2
C35 C 0.2984(3) 0.2708(8) 0.30764(14) 0.167(3) Uani 1 1 d . . . . .
H35A H 0.3114 0.1955 0.2955 0.201 Uiso 1 1 calc R U . . .
H35B H 0.2693 0.2239 0.3142 0.201 Uiso 1 1 calc R U . . .
C27 C 0.4399(2) -0.1522(7) 0.44233(14) 0.1393(19) Uani 1 1 d . . . . .
H27A H 0.4527 -0.2227 0.4292 0.167 Uiso 1 1 calc R U . . .
H27B H 0.4028 -0.1759 0.4407 0.167 Uiso 1 1 calc R U . . .
C36 C 0.2775(4) 0.3915(9) 0.28845(17) 0.213(4) Uani 1 1 d . . . . .
H36B H 0.2551 0.4526 0.2978 0.319 Uiso 1 1 calc R U . . .
H36C H 0.2570 0.3519 0.2694 0.319 Uiso 1 1 calc R U . . .
H36A H 0.3059 0.4532 0.2849 0.319 Uiso 1 1 calc R U . . .
C40 C 0.5479(4) 0.0244(14) 0.3401(3) 0.279(6) Uani 1 1 d . . . . .
H40A H 0.5460 -0.0723 0.3497 0.418 Uiso 1 1 calc R U . F 1
H40B H 0.5844 0.0497 0.3415 0.418 Uiso 1 1 calc R U . F 1
H40C H 0.5292 0.0184 0.3190 0.418 Uiso 1 1 calc R U . F 1
O3A O 0.4623(3) 0.3264(11) 0.7158(2) 0.058(2) Uani 0.5 1 d . . P G 1
O3B O 0.4722(5) 0.2584(16) 0.7167(3) 0.137(5) Uani 0.5 1 d . . P H 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
F2A C1 1.416(15) . ?
F3A C1 1.257(19) . ?
F5A C5 1.238(8) . ?
F6A C5 1.255(10) . ?
F7A C20 1.240(11) . ?
F8A C20 1.261(16) . ?
F9A C20 1.268(13) . ?
F11A C23 1.285(11) . ?
F12A C23 1.152(17) . ?
F2B C1 1.173(11) . ?
F3B C1 1.27(2) . ?
F5B C5 1.310(12) . ?
F6B C5 1.269(11) . ?
F7B C20 1.328(11) . ?
F8B C20 1.326(12) . ?
F9B C20 1.308(12) . ?
F11B C23 1.291(14) . ?
F12B C23 1.362(17) . ?
O2 C16 1.207(4) . ?
O1 C9 1.207(4) . ?
N3 C16 1.363(4) . ?
N3 C14 1.401(4) . ?
N4 C16 1.382(4) . ?
N4 C17 1.393(4) . ?
N2 C9 1.360(4) . ?
N2 C10 1.397(4) . ?
N5 C37 1.502(5) . ?
N5 C33 1.516(5) . ?
N5 C29 1.531(5) . ?
N5 C25 1.542(5) . ?
F1 C1 1.305(7) . ?
F10 C23 1.304(6) . ?
C14 C13 1.377(5) . ?
C14 C15 1.384(4) . ?
N1 C9 1.368(4) . ?
N1 C7 1.396(4) . ?
C10 C15 1.385(4) . ?
C10 C11 1.398(5) . ?
F4 C5 1.296(5) . ?
C17 C18 1.379(4) . ?
C17 C24 1.388(5) . ?
C24 C22 1.348(5) . ?
C7 C6 1.382(5) . ?
C7 C8 1.392(4) . ?
C22 C21 1.404(5) . ?
C22 C23 1.481(6) . ?
C4 C3 1.384(5) . ?
C4 C6 1.388(5) . ?
C4 C5 1.489(6) . ?
C8 C2 1.376(5) . ?
C13 C12 1.371(5) . ?
C11 C12 1.358(5) . ?
C19 C18 1.369(5) . ?
C19 C21 1.382(5) . ?
C19 C20 1.478(6) . ?
C29 C30 1.489(6) . ?
C2 C3 1.388(6) . ?
C2 C1 1.471(6) . ?
C28 C27 1.545(9) . ?
C33 C34 1.487(6) . ?
C25 C26 1.487(6) . ?
C37 C38 1.510(6) . ?
C26 C27 1.530(7) . ?
C34 C35 1.527(7) . ?
C31 C32 1.481(8) . ?
C31 C30 1.514(7) . ?
C38 C39A 1.622(12) . ?
C38 C39B 1.63(2) . ?
C39A C40 1.241(15) . ?
C39B C40 1.385(19) . ?
C35 C36 1.392(8) . ?

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
C16 N3 C14 126.6(3) . . ?
C16 N4 C17 126.1(3) . . ?
C9 N2 C10 128.3(3) . . ?
C37 N5 C33 112.9(3) . . ?
C37 N5 C29 106.1(3) . . ?
C33 N5 C29 110.7(3) . . ?
C37 N5 C25 110.8(3) . . ?
C33 N5 C25 106.0(3) . . ?
C29 N5 C25 110.4(3) . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 N3 117.3(3) . . ?
C15 C14 N3 122.5(3) . . ?
O2 C16 N3 124.6(3) . . ?
O2 C16 N4 122.9(3) . . ?
N3 C16 N4 112.6(3) . . ?
C9 N1 C7 127.0(3) . . ?
C15 C10 N2 123.9(3) . . ?
C15 C10 C11 119.8(3) . . ?
N2 C10 C11 116.3(3) . . ?
C14 C15 C10 119.7(3) . . ?
O1 C9 N2 124.0(3) . . ?
O1 C9 N1 123.3(3) . . ?
N2 C9 N1 112.8(3) . . ?
C18 C17 C24 118.4(3) . . ?
C18 C17 N4 123.5(3) . . ?
C24 C17 N4 118.1(3) . . ?
C22 C24 C17 121.5(3) . . ?
C6 C7 C8 119.5(3) . . ?
C6 C7 N1 123.1(3) . . ?
C8 C7 N1 117.4(3) . . ?
C24 C22 C21 120.5(3) . . ?
C24 C22 C23 120.9(4) . . ?
C21 C22 C23 118.6(4) . . ?
C3 C4 C6 121.2(4) . . ?
C3 C4 C5 121.3(4) . . ?
C6 C4 C5 117.5(4) . . ?
C7 C6 C4 119.6(3) . . ?
C2 C8 C7 120.4(4) . . ?
C12 C13 C14 119.5(3) . . ?
C12 C11 C10 119.1(3) . . ?
C18 C19 C21 121.2(3) . . ?
C18 C19 C20 119.2(4) . . ?
C21 C19 C20 119.6(4) . . ?
C30 C29 N5 117.0(3) . . ?
C19 C18 C17 120.5(3) . . ?
C8 C2 C3 120.6(3) . . ?
C8 C2 C1 119.7(4) . . ?
C3 C2 C1 119.6(4) . . ?
C19 C21 C22 117.9(3) . . ?
C4 C3 C2 118.7(3) . . ?
C11 C12 C13 121.8(3) . . ?
F2B C1 F3B 114.9(13) . . ?
F2B C1 F1 84.6(8) . . ?
F3A C1 F1 89.3(9) . . ?
F3B C1 F1 118.6(8) . . ?
F3A C1 F2A 104.9(14) . . ?
F1 C1 F2A 115.3(7) . . ?
F2B C1 C2 115.7(7) . . ?
F3A C1 C2 119.2(10) . . ?
F3B C1 C2 109.6(9) . . ?
F1 C1 C2 111.7(5) . . ?
F2A C1 C2 114.1(7) . . ?
F5A C5 F6A 112.8(9) . . ?
F5A C5 F4 117.9(6) . . ?
F6A C5 F4 87.5(7) . . ?
F6B C5 F4 114.7(8) . . ?
F6B C5 F5B 114.2(11) . . ?
F4 C5 F5B 81.8(7) . . ?
F5A C5 C4 114.9(5) . . ?
F6A C5 C4 108.2(7) . . ?
F6B C5 C4 115.9(6) . . ?
F4 C5 C4 112.0(4) . . ?
F5B C5 C4 113.5(7) . . ?
F12A C23 F11A 102.1(14) . . ?
F12A C23 F10 92.7(11) . . ?
F11A C23 F10 115.0(9) . . ?
F11B C23 F10 92.7(9) . . ?
F11B C23 F12B 116.7(10) . . ?
F10 C23 F12B 108.1(8) . . ?
F12A C23 C22 115.8(9) . . ?
F11A C23 C22 116.7(7) . . ?
F11B C23 C22 114.7(8) . . ?
F10 C23 C22 111.8(4) . . ?
F12B C23 C22 111.2(7) . . ?
F7A C20 F9A 108.6(12) . . ?
F7A C20 F8A 102.2(13) . . ?
F9A C20 F8A 105.4(12) . . ?
F9B C20 F7B 104.3(9) . . ?
F9B C20 F8B 106.3(11) . . ?
F7B C20 F8B 106.8(12) . . ?
F7A C20 C19 116.4(6) . . ?
F9A C20 C19 113.1(8) . . ?
F8A C20 C19 109.9(8) . . ?
F9B C20 C19 114.2(7) . . ?
F7B C20 C19 110.7(6) . . ?
F8B C20 C19 113.9(6) . . ?
C34 C33 N5 116.4(3) . . ?
C26 C25 N5 117.3(3) . . ?
N5 C37 C38 116.1(3) . . ?
C25 C26 C27 107.6(4) . . ?
C33 C34 C35 112.3(4) . . ?
C32 C31 C30 114.5(5) . . ?
C37 C38 C39A 103.2(5) . . ?
C37 C38 C39B 112.3(7) . . ?
C29 C30 C31 111.4(4) . . ?
C40 C39A C38 110.8(9) . . ?
C40 C39B C38 103.2(17) . . ?
C36 C35 C34 119.9(6) . . ?
C26 C27 C28 115.5(6) . . ?

_refine_diff_density_max         0.601
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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_L-TBAHCO3
_database_code_depnum_ccdc_archive 'CCDC 1551281'
_audit_update_record             
;
2017-05-20 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H14 F12 N4 O2, 2(C16 H36 N), 2(C H O3)'
_chemical_formula_sum            'C58 H88 F12 N6 O8'
_chemical_formula_weight         1225.34

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.5913(19)
_cell_length_b                   22.1973(14)
_cell_length_c                   16.0329(14)
_cell_angle_alpha                90
_cell_angle_beta                 102.823(9)
_cell_angle_gamma                90
_cell_volume                     6798.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4330
_cell_measurement_theta_min      3.2810
_cell_measurement_theta_max      22.5080

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_F_000             2600.0
_exptl_transmission_factor_min   0.973
_exptl_transmission_factor_max   0.982
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.101
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39758
_diffrn_reflns_av_unetI/netI     0.1194
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.046
_diffrn_reflns_theta_max         28.816
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             16771
_reflns_number_gt                9160
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+0.0010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         16771
_refine_ls_number_parameters     764
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.2980
_refine_ls_R_factor_gt           0.1262
_refine_ls_wR_factor_ref         0.3616
_refine_ls_wR_factor_gt          0.2939
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.003

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
C15 C 0.86716(12) 0.00321(14) 0.20799(18) 0.0697(11) Uani 1 1 d G . . . .
H15 H 0.8185 0.0039 0.1927 0.084 Uiso 1 1 calc R U . . .
C10 C 0.90557(17) 0.04825(11) 0.17924(16) 0.0689(11) Uani 1 1 d G . . . .
C11 C 0.97827(17) 0.04725(13) 0.20204(19) 0.0814(13) Uani 1 1 d G . . . .
H11 H 1.0040 0.0774 0.1828 0.098 Uiso 1 1 calc R U . . .
C12 C 1.01257(12) 0.00122(16) 0.2536(2) 0.0926(15) Uani 1 1 d G . . . .
H12 H 1.0612 0.0005 0.2688 0.111 Uiso 1 1 calc R U . . .
C13 C 0.97416(18) -0.04382(13) 0.28232(17) 0.0858(13) Uani 1 1 d G . . . .
H13 H 0.9971 -0.0746 0.3168 0.103 Uiso 1 1 calc R U . . .
C14 C 0.90146(17) -0.04282(11) 0.25953(17) 0.0717(12) Uani 1 1 d G . . . .
C32 C 0.2168(12) 0.8524(6) 0.2853(11) 0.64(2) Uani 1 1 d D . . . .
H32A H 0.2479 0.8445 0.3394 0.961 Uiso 1 1 calc R U . . .
H22B H 0.1696 0.8437 0.2892 0.961 Uiso 1 1 calc R U . . .
H32B H 0.2204 0.8940 0.2704 0.961 Uiso 1 1 calc R U . . .
C4 C 0.6102(3) 0.1254(3) -0.1078(3) 0.154(3) Uani 1 1 d G . . . .
C6 C 0.6772(3) 0.11316(18) -0.0604(3) 0.1164(18) Uani 1 1 d G . . . .
H6 H 0.6982 0.0763 -0.0665 0.140 Uiso 1 1 calc R U . . .
C7 C 0.71285(18) 0.1560(2) -0.0039(2) 0.0962(15) Uani 1 1 d G . . . .
C8 C 0.6815(3) 0.21102(19) 0.0053(2) 0.1020(17) Uani 1 1 d G . . . .
H8 H 0.7053 0.2397 0.0432 0.122 Uiso 1 1 calc R U . . .
C2 C 0.6145(3) 0.2233(2) -0.0421(3) 0.134(2) Uani 1 1 d G . . . .
C3 C 0.57882(18) 0.1804(3) -0.0987(3) 0.165(3) Uani 1 1 d G . . . .
H3 H 0.5340 0.1886 -0.1304 0.198 Uiso 1 1 calc R U . . .
F7 F 0.5731(6) -0.0094(3) 0.3985(7) 0.317(6) Uani 1 1 d . . . . .
F10 F 0.6115(4) -0.3102(3) 0.3168(7) 0.249(3) Uani 1 1 d . . . . .
F11 F 0.5591(4) -0.2921(3) 0.3929(5) 0.263(3) Uani 1 1 d . . . . .
F12A F 0.5070(4) -0.2654(4) 0.2889(7) 0.212(4) Uani 0.7 1 d . . P . .
F8 F 0.5984(4) -0.0485(4) 0.5057(5) 0.309(5) Uani 1 1 d . . . . .
F9 F 0.5078(3) -0.0680(3) 0.4346(6) 0.285(4) Uani 1 1 d . . . . .
F4 F 0.5738(6) 0.0296(4) -0.1377(7) 0.350(7) Uani 1 1 d . . . . .
F5 F 0.6033(5) 0.0775(5) -0.2330(6) 0.354(6) Uani 1 1 d . . . . .
F6 F 0.5119(3) 0.0914(3) -0.2016(4) 0.274(3) Uani 1 1 d . . . . .
O1 O 0.77812(18) 0.04341(15) 0.0535(2) 0.1022(11) Uani 1 1 d . . . . .
O2 O 0.77094(19) -0.03438(17) 0.3073(2) 0.1063(12) Uani 1 1 d . . . . .
N4 N 0.7712(2) -0.13591(19) 0.3244(3) 0.0973(12) Uani 1 1 d . . . . .
H4N H 0.7961 -0.1679 0.3250 0.117 Uiso 1 1 calc R U . . .
N3 N 0.8643(2) -0.08949(16) 0.2886(2) 0.0808(11) Uani 1 1 d . . . . .
H3N H 0.8834 -0.1246 0.2954 0.097 Uiso 1 1 calc R U . . .
N2 N 0.8713(2) 0.09591(16) 0.1294(2) 0.0797(10) Uani 1 1 d . . . . .
H2N H 0.8918 0.1304 0.1343 0.096 Uiso 1 1 calc R U . . .
N1 N 0.7812(2) 0.14683(18) 0.0467(2) 0.0908(12) Uani 1 1 d . . . . .
H1N H 0.8074 0.1779 0.0609 0.109 Uiso 1 1 calc R U . . .
C9 C 0.8082(3) 0.0915(2) 0.0743(3) 0.0759(12) Uani 1 1 d . . . . .
C16 C 0.7998(3) -0.0829(2) 0.3068(3) 0.0879(15) Uani 1 1 d . . . . .
C17 C 0.7046(3) -0.1429(3) 0.3418(3) 0.0888(14) Uani 1 1 d . . . . .
C24 C 0.6733(3) -0.1993(3) 0.3269(3) 0.0976(15) Uani 1 1 d . . . . .
H24 H 0.6958 -0.2308 0.3056 0.117 Uiso 1 1 calc R U . . .
C18 C 0.6710(3) -0.0971(3) 0.3764(3) 0.1062(17) Uani 1 1 d . . . . .
H18 H 0.6923 -0.0597 0.3876 0.127 Uiso 1 1 calc R U . . .
C20 C 0.5672(7) -0.0585(6) 0.4273(9) 0.182(4) Uani 1 1 d . . . . .
C22 C 0.6074(4) -0.2074(4) 0.3446(4) 0.1120(18) Uani 1 1 d . . . . .
C21 C 0.5749(3) -0.1625(4) 0.3795(4) 0.127(2) Uani 1 1 d . . . . .
H21 H 0.5319 -0.1695 0.3932 0.152 Uiso 1 1 calc R U . . .
C19 C 0.6065(4) -0.1068(4) 0.3941(4) 0.121(2) Uani 1 1 d . . . . .
C5 C 0.5756(6) 0.0779(8) -0.1683(8) 0.210(6) Uani 1 1 d . . . . .
N5 N 0.1889(3) 0.6491(2) 0.1284(3) 0.1259(17) Uani 1 1 d . . . . .
C25 C 0.1132(4) 0.6390(3) 0.1347(4) 0.149(3) Uani 1 1 d . . . . .
H25A H 0.1069 0.6550 0.1887 0.179 Uiso 1 1 calc R U . . .
H25B H 0.1043 0.5960 0.1346 0.179 Uiso 1 1 calc R U . . .
C37 C 0.2028(4) 0.6270(3) 0.0459(3) 0.130(2) Uani 1 1 d . . . . .
H37A H 0.2520 0.6330 0.0468 0.156 Uiso 1 1 calc R U . . .
H37B H 0.1760 0.6514 -0.0002 0.156 Uiso 1 1 calc R U . . .
C33 C 0.2335(5) 0.6158(3) 0.2037(4) 0.139(2) Uani 1 1 d . . . . .
H33A H 0.2214 0.6303 0.2556 0.167 Uiso 1 1 calc R U . . .
H33B H 0.2212 0.5734 0.1982 0.167 Uiso 1 1 calc R U . . .
C38 C 0.1849(5) 0.5613(3) 0.0262(4) 0.174(3) Uani 1 1 d . . . . .
H38B H 0.2101 0.5363 0.0725 0.209 Uiso 1 1 calc R U . . .
H38A H 0.1352 0.5550 0.0210 0.209 Uiso 1 1 calc R U . . .
C40 C 0.1869(8) 0.4764(4) -0.0679(7) 0.374(9) Uani 1 1 d D . . . .
H40A H 0.1995 0.4564 -0.0136 0.560 Uiso 1 1 calc R U . . .
H40B H 0.2125 0.4591 -0.1065 0.560 Uiso 1 1 calc R U . . .
H90C H 0.1376 0.4718 -0.0909 0.560 Uiso 1 1 calc R U . . .
C35 C 0.3453(5) 0.5869(5) 0.2954(6) 0.219(4) Uani 1 1 d D . . . .
H35A H 0.3319 0.5448 0.2887 0.262 Uiso 1 1 calc R U . . .
H35B H 0.3280 0.6028 0.3431 0.262 Uiso 1 1 calc R U . . .
C36 C 0.4258(5) 0.5911(5) 0.3170(9) 0.339(9) Uani 1 1 d D . . . .
H36B H 0.4428 0.5855 0.2658 0.508 Uiso 1 1 calc R U . . .
H58 H 0.4448 0.5604 0.3577 0.508 Uiso 1 1 calc R U . . .
H36A H 0.4399 0.6300 0.3409 0.508 Uiso 1 1 calc R U . . .
C29 C 0.2069(4) 0.7155(3) 0.1311(4) 0.151(3) Uani 1 1 d . . . . .
H29A H 0.1798 0.7343 0.0797 0.181 Uiso 1 1 calc R U . . .
H29B H 0.2559 0.7196 0.1297 0.181 Uiso 1 1 calc R U . . .
C30 C 0.1938(5) 0.7502(3) 0.2093(5) 0.201(4) Uani 1 1 d . . . . .
H30A H 0.2095 0.7266 0.2609 0.241 Uiso 1 1 calc R U . . .
H30B H 0.1442 0.7584 0.2025 0.241 Uiso 1 1 calc R U . . .
C34 C 0.3102(5) 0.6209(4) 0.2143(5) 0.180(3) Uani 1 1 d . . . . .
H34A H 0.3240 0.6629 0.2190 0.215 Uiso 1 1 calc R U . . .
H34B H 0.3243 0.6038 0.1650 0.215 Uiso 1 1 calc R U . . .
N6 N 0.1893(3) 0.3556(2) 0.4848(3) 0.1168(15) Uani 1 1 d . . . . .
C55 C 0.3504(6) 0.4283(5) 0.4208(7) 0.228(5) Uani 1 1 d D . . . .
H55A H 0.3312 0.4688 0.4158 0.274 Uiso 1 1 calc R U . . .
H55B H 0.3451 0.4113 0.3640 0.274 Uiso 1 1 calc R U . . .
C56 C 0.4277(6) 0.4286(8) 0.4686(9) 0.418(13) Uani 1 1 d D . . . .
H56A H 0.4354 0.3976 0.5115 0.627 Uiso 1 1 calc R U . . .
H56B H 0.4392 0.4671 0.4953 0.627 Uiso 1 1 calc R U . . .
H56C H 0.4569 0.4212 0.4287 0.627 Uiso 1 1 calc R U . . .
C49 C 0.2005(4) 0.3747(3) 0.5777(3) 0.130(2) Uani 1 1 d . . . . .
H49A H 0.1725 0.3489 0.6058 0.156 Uiso 1 1 calc R U . . .
H49B H 0.2492 0.3681 0.6052 0.156 Uiso 1 1 calc R U . . .
C41 C 0.2067(4) 0.2888(3) 0.4875(3) 0.131(2) Uani 1 1 d . . . . .
H41B H 0.2552 0.2835 0.5168 0.157 Uiso 1 1 calc R U . . .
H41A H 0.1779 0.2682 0.5206 0.157 Uiso 1 1 calc R U . . .
C45 C 0.1141(4) 0.3663(3) 0.4370(4) 0.139(2) Uani 1 1 d . . . . .
H45A H 0.1051 0.4093 0.4361 0.167 Uiso 1 1 calc R U . . .
H45B H 0.1097 0.3535 0.3782 0.167 Uiso 1 1 calc R U . . .
C54 C 0.3139(5) 0.3888(4) 0.4761(6) 0.185(3) Uani 1 1 d . . . . .
H54A H 0.3246 0.4032 0.5347 0.222 Uiso 1 1 calc R U . . .
H54B H 0.3299 0.3475 0.4757 0.222 Uiso 1 1 calc R U . . .
C46 C 0.0584(5) 0.3355(4) 0.4713(5) 0.175(3) Uani 1 1 d . . . . .
H46B H 0.0638 0.3461 0.5311 0.210 Uiso 1 1 calc R U . . .
H46A H 0.0645 0.2922 0.4681 0.210 Uiso 1 1 calc R U . . .
C50 C 0.1824(4) 0.4392(3) 0.5919(4) 0.169(3) Uani 1 1 d D . . . .
H50A H 0.1326 0.4454 0.5695 0.203 Uiso 1 1 calc R U . . .
H50B H 0.2075 0.4655 0.5608 0.203 Uiso 1 1 calc R U . . .
C47 C -0.0145(6) 0.3518(4) 0.4237(6) 0.203(4) Uani 1 1 d D . . . .
H47A H -0.0469 0.3226 0.4379 0.244 Uiso 1 1 calc R U . . .
H47B H -0.0167 0.3486 0.3628 0.244 Uiso 1 1 calc R U . . .
C48 C -0.0388(6) 0.4153(5) 0.4426(6) 0.237(5) Uani 1 1 d D . . . .
H48B H -0.0006 0.4431 0.4470 0.356 Uiso 1 1 calc R U . . .
H48A H -0.0540 0.4148 0.4955 0.356 Uiso 1 1 calc R U . . .
H48C H -0.0768 0.4276 0.3971 0.356 Uiso 1 1 calc R U . . .
C51 C 0.2010(5) 0.4559(4) 0.6875(4) 0.197(4) Uani 1 1 d D . . . .
H51B H 0.1846 0.4965 0.6944 0.237 Uiso 1 1 calc R U . . .
H51A H 0.1768 0.4288 0.7185 0.237 Uiso 1 1 calc R U . . .
C42 C 0.1954(5) 0.2601(3) 0.4005(4) 0.191(4) Uani 1 1 d . . . . .
H42A H 0.2210 0.2818 0.3648 0.229 Uiso 1 1 calc R U . . .
H42B H 0.1461 0.2606 0.3727 0.229 Uiso 1 1 calc R U . . .
C52 C 0.2802(5) 0.4527(8) 0.7264(9) 0.415(13) Uani 1 1 d D . . . .
H52B H 0.2997 0.4183 0.7039 0.623 Uiso 1 1 calc R U . . .
H52A H 0.2879 0.4492 0.7875 0.623 Uiso 1 1 calc R U . . .
H52C H 0.3024 0.4887 0.7122 0.623 Uiso 1 1 calc R U . . .
C53 C 0.2345(4) 0.3923(3) 0.4384(4) 0.133(2) Uani 1 1 d . . . . .
H53A H 0.2201 0.4342 0.4382 0.160 Uiso 1 1 calc R U . . .
H53B H 0.2255 0.3790 0.3794 0.160 Uiso 1 1 calc R U . . .
O7 O 0.0718(2) 0.29831(16) 0.2018(3) 0.1138(13) Uani 1 1 d . . . . .
O8 O 0.07373(19) 0.19886(15) 0.1835(2) 0.1096(12) Uani 1 1 d . . . . .
H8O H 0.0266 0.2072 0.1961 0.164 Uiso 1 1 d R U . . .
O6 O 0.1684(2) 0.25235(15) 0.1853(2) 0.1110(12) Uani 1 1 d . . . . .
C58 C 0.1052(4) 0.2520(3) 0.1907(3) 0.0937(15) Uani 1 1 d . . . . .
O3 O 0.8420(2) 0.25559(16) 0.0942(2) 0.1113(12) Uani 1 1 d . . . . .
O5 O 0.9362(3) 0.30740(15) 0.1474(2) 0.1094(12) Uani 1 1 d . . . . .
O4 O 0.93803(19) 0.20784(16) 0.1617(2) 0.1082(12) Uani 1 1 d . . . . .
C57 C 0.9045(4) 0.2544(3) 0.1331(4) 0.0911(15) Uani 1 1 d . . . . .
C43 C 0.2226(6) 0.1933(4) 0.4140(6) 0.254(6) Uani 1 1 d D . . . .
H43A H 0.2266 0.1811 0.4730 0.304 Uiso 1 1 calc R U . . .
H43B H 0.1907 0.1661 0.3772 0.304 Uiso 1 1 calc R U . . .
C44 C 0.2948(7) 0.1927(7) 0.3911(10) 0.396(12) Uani 1 1 d D . . . .
H44A H 0.2976 0.2252 0.3525 0.594 Uiso 1 1 calc R U . . .
H44C H 0.3012 0.1551 0.3641 0.594 Uiso 1 1 calc R U . . .
H44B H 0.3307 0.1973 0.4422 0.594 Uiso 1 1 calc R U . . .
C26 C 0.0587(6) 0.6685(4) 0.0610(5) 0.190(4) Uani 1 1 d . . . . .
H26B H 0.0668 0.6555 0.0063 0.228 Uiso 1 1 calc R U . . .
H26A H 0.0632 0.7120 0.0644 0.228 Uiso 1 1 calc R U . . .
C27 C -0.0176(6) 0.6492(5) 0.0689(7) 0.218(4) Uani 1 1 d D . . . .
H27B H -0.0180 0.6460 0.1291 0.261 Uiso 1 1 calc R U . . .
H27A H -0.0499 0.6812 0.0450 0.261 Uiso 1 1 calc R U . . .
C39 C 0.2047(6) 0.5439(4) -0.0560(6) 0.223(5) Uani 1 1 d D . . . .
H39B H 0.2542 0.5506 -0.0522 0.267 Uiso 1 1 calc R U . . .
H39A H 0.1781 0.5671 -0.1035 0.267 Uiso 1 1 calc R U . . .
C23 C 0.5669(7) -0.2649(4) 0.3167(10) 0.176(4) Uani 1 1 d . . . . .
C31 C 0.2367(8) 0.8123(4) 0.2161(7) 0.313(8) Uani 1 1 d D . . . .
H31B H 0.2866 0.8040 0.2307 0.375 Uiso 1 1 calc R U . . .
H31A H 0.2260 0.8329 0.1614 0.375 Uiso 1 1 calc R U . . .
F1 F 0.5868(5) 0.2965(4) 0.0455(6) 0.308(5) Uani 1 1 d . . . . .
F2 F 0.5158(4) 0.2789(4) -0.0472(7) 0.286(3) Uani 1 1 d . . . . .
F3A F 0.5762(7) 0.3154(5) -0.0970(8) 0.238(4) Uani 0.7 1 d . . P . .
F3B F 0.6378(9) 0.3344(7) -0.018(2) 0.178(10) Uani 0.3 1 d . . P . .
C1 C 0.5923(8) 0.2916(9) -0.0294(9) 0.246(9) Uani 1 1 d . . . . .
F12B F 0.5632(9) -0.2802(7) 0.2358(9) 0.141(5) Uani 0.3 1 d . . P . .
C28 C -0.0454(12) 0.5897(7) 0.0248(11) 0.55(2) Uani 1 1 d D . . . .
H28B H -0.0094 0.5710 0.0016 0.829 Uiso 1 1 calc R U . . .
H28A H -0.0854 0.5978 -0.0205 0.829 Uiso 1 1 calc R U . . .
H30C H -0.0586 0.5632 0.0658 0.829 Uiso 1 1 calc R U . . .
H5O H 0.988(3) 0.306(3) 0.163(4) 0.14(2) Uiso 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
C15 C10 1.3900 . ?
C15 C14 1.3900 . ?
C15 H15 0.9300 . ?
C10 C11 1.3900 . ?
C10 N2 1.404(4) . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 N3 1.404(4) . ?
C32 C31 1.5398(7) . ?
C32 H32A 0.9601 . ?
C32 H22B 0.9601 . ?
C32 H32B 0.9601 . ?
C4 C6 1.3900 . ?
C4 C3 1.3900 . ?
C4 C5 1.490(13) . ?
C6 C7 1.3900 . ?
C6 H6 0.9300 . ?
C7 C8 1.3900 . ?
C7 N1 1.418(5) . ?
C8 C2 1.3900 . ?
C8 H8 0.9300 . ?
C2 C3 1.3900 . ?
C2 C1 1.603(17) . ?
C3 H3 0.9300 . ?
F7 C20 1.201(11) . ?
F10 C23 1.332(10) . ?
F11 C23 1.402(13) . ?
F12A C23 1.159(12) . ?
F8 C20 1.289(12) . ?
F9 C20 1.215(11) . ?
F4 C5 1.183(15) . ?
F5 C5 1.273(12) . ?
F6 C5 1.280(11) . ?
O1 C9 1.230(5) . ?
O2 C16 1.217(5) . ?
N4 C16 1.360(6) . ?
N4 C17 1.401(6) . ?
N4 H4N 0.8600 . ?
N3 C16 1.366(6) . ?
N3 H3N 0.8600 . ?
N2 C9 1.353(5) . ?
N2 H2N 0.8600 . ?
N1 C9 1.370(5) . ?
N1 H1N 0.8600 . ?
C17 C24 1.390(7) . ?
C17 C18 1.394(7) . ?
C24 C22 1.394(7) . ?
C24 H24 0.9300 . ?
C18 C19 1.372(7) . ?
C18 H18 0.9300 . ?
C20 C19 1.484(11) . ?
C22 C21 1.367(8) . ?
C22 C23 1.517(12) . ?
C21 C19 1.380(8) . ?
C21 H21 0.9300 . ?
N5 C37 1.493(6) . ?
N5 C29 1.513(7) . ?
N5 C33 1.517(7) . ?
N5 C25 1.526(8) . ?
C25 C26 1.550(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C37 C38 1.515(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C33 C34 1.478(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C38 C39 1.504(10) . ?
C38 H38B 0.9700 . ?
C38 H38A 0.9700 . ?
C40 C39 1.5397(10) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H90C 0.9600 . ?
C35 C34 1.529(10) . ?
C35 C36 1.5395(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36B 0.9600 . ?
C36 H58 0.9601 . ?
C36 H36A 0.9600 . ?
C29 C30 1.542(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.605(10) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
N6 C49 1.517(6) . ?
N6 C53 1.514(7) . ?
N6 C45 1.521(7) . ?
N6 C41 1.520(6) . ?
C55 C54 1.531(10) . ?
C55 C56 1.5392(10) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C49 C50 1.504(8) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C41 C42 1.506(8) . ?
C41 H41B 0.9700 . ?
C41 H41A 0.9700 . ?
C45 C46 1.492(8) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C54 C53 1.541(9) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C46 C47 1.506(10) . ?
C46 H46B 0.9700 . ?
C46 H46A 0.9700 . ?
C50 C51 1.5398(10) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C47 C48 1.5392(10) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48B 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48C 0.9600 . ?
C51 C52 1.5395(11) . ?
C51 H51B 0.9700 . ?
C51 H51A 0.9700 . ?
C42 C43 1.573(10) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C52 H52B 0.9602 . ?
C52 H52A 0.9602 . ?
C52 H52C 0.9602 . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
O7 C58 1.253(6) . ?
O8 C58 1.324(6) . ?
O8 H8O 1.0041 . ?
O6 C58 1.261(6) . ?
O3 C57 1.245(6) . ?
O5 C57 1.327(6) . ?
O5 H5O 0.99(6) . ?
O4 C57 1.255(6) . ?
C43 C44 1.5391(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9607 . ?
C44 H44C 0.9607 . ?
C44 H44B 0.9607 . ?
C26 C27 1.586(11) . ?
C26 H26B 0.9700 . ?
C26 H26A 0.9700 . ?
C27 C28 1.5391(11) . ?
C27 H27B 0.9700 . ?
C27 H27A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39A 0.9700 . ?
C23 F12B 1.326(16) . ?
C31 H31B 0.9700 . ?
C31 H31A 0.9700 . ?
F1 C1 1.233(12) . ?
F2 C1 1.488(18) . ?
F3A C1 1.184(12) . ?
F3B C1 1.29(2) . ?
C28 H28B 1.1233 . ?
C28 H28A 1.1357 . ?
C28 H30C 1.1193 . ?

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
C10 C15 C14 120.0 . . ?
C10 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C10 C11 120.0 . . ?
C15 C10 N2 120.3(3) . . ?
C11 C10 N2 119.7(3) . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 N3 118.5(3) . . ?
C15 C14 N3 121.4(3) . . ?
C31 C32 H32A 109.8 . . ?
C31 C32 H22B 109.2 . . ?
H32A C32 H22B 109.5 . . ?
C31 C32 H32B 109.4 . . ?
H32A C32 H32B 109.5 . . ?
H22B C32 H32B 109.5 . . ?
C6 C4 C3 120.0 . . ?
C6 C4 C5 117.1(7) . . ?
C3 C4 C5 122.9(7) . . ?
C7 C6 C4 120.0 . . ?
C7 C6 H6 120.0 . . ?
C4 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 N1 116.7(4) . . ?
C6 C7 N1 123.3(4) . . ?
C7 C8 C2 120.0 . . ?
C7 C8 H8 120.0 . . ?
C2 C8 H8 120.0 . . ?
C8 C2 C3 120.0 . . ?
C8 C2 C1 111.4(7) . . ?
C3 C2 C1 128.2(7) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C16 N4 C17 125.6(5) . . ?
C16 N4 H4N 117.2 . . ?
C17 N4 H4N 117.2 . . ?
C16 N3 C14 124.4(4) . . ?
C16 N3 H3N 117.8 . . ?
C14 N3 H3N 117.8 . . ?
C9 N2 C10 124.7(4) . . ?
C9 N2 H2N 117.6 . . ?
C10 N2 H2N 117.6 . . ?
C9 N1 C7 124.1(4) . . ?
C9 N1 H1N 118.0 . . ?
C7 N1 H1N 117.9 . . ?
O1 C9 N2 123.5(4) . . ?
O1 C9 N1 124.3(5) . . ?
N2 C9 N1 112.2(4) . . ?
O2 C16 N4 123.5(5) . . ?
O2 C16 N3 123.3(5) . . ?
N4 C16 N3 113.2(5) . . ?
C24 C17 C18 119.7(5) . . ?
C24 C17 N4 117.4(5) . . ?
C18 C17 N4 122.8(5) . . ?
C17 C24 C22 118.4(6) . . ?
C17 C24 H24 120.8 . . ?
C22 C24 H24 120.8 . . ?
C19 C18 C17 120.5(6) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.7 . . ?
F7 C20 F9 111.7(14) . . ?
F7 C20 F8 98.8(11) . . ?
F9 C20 F8 101.2(9) . . ?
F7 C20 C19 114.6(9) . . ?
F9 C20 C19 119.6(10) . . ?
F8 C20 C19 107.6(12) . . ?
C21 C22 C24 121.7(6) . . ?
C21 C22 C23 118.2(8) . . ?
C24 C22 C23 119.8(8) . . ?
C22 C21 C19 119.4(7) . . ?
C22 C21 H21 120.3 . . ?
C19 C21 H21 120.3 . . ?
C18 C19 C21 120.2(7) . . ?
C18 C19 C20 122.4(8) . . ?
C21 C19 C20 117.4(8) . . ?
F4 C5 F5 112.9(17) . . ?
F4 C5 F6 105.7(12) . . ?
F5 C5 F6 102.4(11) . . ?
F4 C5 C4 115.0(11) . . ?
F5 C5 C4 108.7(11) . . ?
F6 C5 C4 111.4(12) . . ?
C37 N5 C29 105.0(4) . . ?
C37 N5 C33 111.0(5) . . ?
C29 N5 C33 111.3(5) . . ?
C37 N5 C25 112.3(5) . . ?
C29 N5 C25 111.5(5) . . ?
C33 N5 C25 105.8(5) . . ?
N5 C25 C26 113.8(6) . . ?
N5 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
N5 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N5 C37 C38 115.1(5) . . ?
N5 C37 H37A 108.5 . . ?
C38 C37 H37A 108.5 . . ?
N5 C37 H37B 108.5 . . ?
C38 C37 H37B 108.5 . . ?
H37A C37 H37B 107.5 . . ?
C34 C33 N5 116.4(6) . . ?
C34 C33 H33A 108.2 . . ?
N5 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
N5 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C39 C38 C37 109.8(6) . . ?
C39 C38 H38B 109.7 . . ?
C37 C38 H38B 109.7 . . ?
C39 C38 H38A 109.8 . . ?
C37 C38 H38A 109.7 . . ?
H38B C38 H38A 108.2 . . ?
C39 C40 H40A 109.6 . . ?
C39 C40 H40B 109.6 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H90C 109.3 . . ?
H40A C40 H90C 109.5 . . ?
H40B C40 H90C 109.5 . . ?
C34 C35 C36 114.0(9) . . ?
C34 C35 H35A 108.7 . . ?
C36 C35 H35A 108.7 . . ?
C34 C35 H35B 108.8 . . ?
C36 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H58 109.6 . . ?
H36B C36 H58 109.5 . . ?
C35 C36 H36A 109.4 . . ?
H36B C36 H36A 109.5 . . ?
H58 C36 H36A 109.5 . . ?
N5 C29 C30 115.5(5) . . ?
N5 C29 H29A 108.3 . . ?
C30 C29 H29A 108.5 . . ?
N5 C29 H29B 108.5 . . ?
C30 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 C31 107.7(6) . . ?
C29 C30 H30A 110.2 . . ?
C31 C30 H30A 110.2 . . ?
C29 C30 H30B 110.1 . . ?
C31 C30 H30B 110.1 . . ?
H30A C30 H30B 108.5 . . ?
C33 C34 C35 108.3(7) . . ?
C33 C34 H34A 110.0 . . ?
C35 C34 H34A 110.0 . . ?
C33 C34 H34B 110.1 . . ?
C35 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
C49 N6 C53 111.1(5) . . ?
C49 N6 C45 111.4(5) . . ?
C53 N6 C45 106.0(5) . . ?
C49 N6 C41 105.2(4) . . ?
C53 N6 C41 112.8(5) . . ?
C45 N6 C41 110.6(5) . . ?
C54 C55 C56 104.4(8) . . ?
C54 C55 H55A 110.9 . . ?
C56 C55 H55A 111.0 . . ?
C54 C55 H55B 110.8 . . ?
C56 C55 H55B 110.8 . . ?
H55A C55 H55B 108.9 . . ?
C55 C56 H56A 109.4 . . ?
C55 C56 H56B 109.4 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.6 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C50 C49 N6 115.2(5) . . ?
C50 C49 H49A 108.5 . . ?
N6 C49 H49A 108.5 . . ?
C50 C49 H49B 108.5 . . ?
N6 C49 H49B 108.4 . . ?
H49A C49 H49B 107.5 . . ?
C42 C41 N6 113.6(5) . . ?
C42 C41 H41B 108.8 . . ?
N6 C41 H41B 108.9 . . ?
C42 C41 H41A 108.9 . . ?
N6 C41 H41A 108.8 . . ?
H41B C41 H41A 107.7 . . ?
C46 C45 N6 116.7(6) . . ?
C46 C45 H45A 108.1 . . ?
N6 C45 H45A 108.1 . . ?
C46 C45 H45B 108.2 . . ?
N6 C45 H45B 108.1 . . ?
H45A C45 H45B 107.3 . . ?
C55 C54 C53 107.7(7) . . ?
C55 C54 H54A 110.0 . . ?
C53 C54 H54A 110.2 . . ?
C55 C54 H54B 110.2 . . ?
C53 C54 H54B 110.2 . . ?
H54A C54 H54B 108.5 . . ?
C45 C46 C47 113.0(7) . . ?
C45 C46 H46B 109.0 . . ?
C47 C46 H46B 108.9 . . ?
C45 C46 H46A 109.0 . . ?
C47 C46 H46A 109.0 . . ?
H46B C46 H46A 107.8 . . ?
C49 C50 C51 111.6(6) . . ?
C49 C50 H50A 109.3 . . ?
C51 C50 H50A 109.3 . . ?
C49 C50 H50B 109.3 . . ?
C51 C50 H50B 109.3 . . ?
H50A C50 H50B 108.0 . . ?
C46 C47 C48 114.8(8) . . ?
C46 C47 H47A 108.6 . . ?
C48 C47 H47A 108.5 . . ?
C46 C47 H47B 108.5 . . ?
C48 C47 H47B 108.6 . . ?
H47A C47 H47B 107.6 . . ?
C47 C48 H48B 109.4 . . ?
C47 C48 H48A 109.5 . . ?
H48B C48 H48A 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
C52 C51 C50 112.8(8) . . ?
C52 C51 H51B 109.1 . . ?
C50 C51 H51B 109.0 . . ?
C52 C51 H51A 109.0 . . ?
C50 C51 H51A 109.0 . . ?
H51B C51 H51A 107.8 . . ?
C41 C42 C43 107.2(6) . . ?
C41 C42 H42A 110.3 . . ?
C43 C42 H42A 110.3 . . ?
C41 C42 H42B 110.2 . . ?
C43 C42 H42B 110.2 . . ?
H42A C42 H42B 108.5 . . ?
C51 C52 H52B 109.6 . . ?
C51 C52 H52A 109.4 . . ?
H52B C52 H52A 109.5 . . ?
C51 C52 H52C 109.4 . . ?
H52B C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
N6 C53 C54 115.4(5) . . ?
N6 C53 H53A 108.4 . . ?
C54 C53 H53A 108.4 . . ?
N6 C53 H53B 108.4 . . ?
C54 C53 H53B 108.4 . . ?
H53A C53 H53B 107.5 . . ?
C58 O8 H8O 104.5 . . ?
O7 C58 O6 123.9(6) . . ?
O7 C58 O8 119.7(6) . . ?
O6 C58 O8 116.4(6) . . ?
C57 O5 H5O 116(4) . . ?
O3 C57 O4 125.3(6) . . ?
O3 C57 O5 116.0(6) . . ?
O4 C57 O5 118.7(6) . . ?
C44 C43 C42 106.1(9) . . ?
C44 C43 H43A 110.4 . . ?
C42 C43 H43A 110.5 . . ?
C44 C43 H43B 110.6 . . ?
C42 C43 H43B 110.6 . . ?
H43A C43 H43B 108.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.4 . . ?
C43 C44 H44B 109.6 . . ?
H44A C44 H44B 109.4 . . ?
H44C C44 H44B 109.4 . . ?
C25 C26 C27 109.1(8) . . ?
C25 C26 H26B 109.8 . . ?
C27 C26 H26B 110.0 . . ?
C25 C26 H26A 109.8 . . ?
C27 C26 H26A 109.9 . . ?
H26B C26 H26A 108.3 . . ?
C28 C27 C26 116.0(11) . . ?
C28 C27 H27B 107.7 . . ?
C26 C27 H27B 108.5 . . ?
C28 C27 H27A 108.6 . . ?
C26 C27 H27A 108.3 . . ?
H27B C27 H27A 107.4 . . ?
C38 C39 C40 105.2(8) . . ?
C38 C39 H39B 110.7 . . ?
C40 C39 H39B 110.5 . . ?
C38 C39 H39A 110.7 . . ?
C40 C39 H39A 110.9 . . ?
H39B C39 H39A 108.8 . . ?
F12A C23 F12B 78.0(15) . . ?
F12A C23 F10 127.0(13) . . ?
F12B C23 F10 72.6(11) . . ?
F12A C23 F11 91.9(9) . . ?
F12B C23 F11 138.5(11) . . ?
F10 C23 F11 82.7(9) . . ?
F12A C23 C22 122.7(10) . . ?
F12B C23 C22 114.5(9) . . ?
F10 C23 C22 109.5(10) . . ?
F11 C23 C22 104.9(11) . . ?
C32 C31 C30 109.4(9) . . ?
C32 C31 H31B 109.6 . . ?
C30 C31 H31B 109.7 . . ?
C32 C31 H31A 110.0 . . ?
C30 C31 H31A 109.9 . . ?
H31B C31 H31A 108.3 . . ?
F3A C1 F1 142.1(14) . . ?
F3A C1 F3B 80.3(18) . . ?
F1 C1 F3B 91(2) . . ?
F3A C1 F2 81.7(13) . . ?
F1 C1 F2 84.4(9) . . ?
F3B C1 F2 143.4(16) . . ?
F3A C1 C2 109.3(12) . . ?
F1 C1 C2 107.0(12) . . ?
F3B C1 C2 121.0(10) . . ?
F2 C1 C2 95.0(13) . . ?
C27 C28 H28B 125.5 . . ?
C27 C28 H28A 126.7 . . ?
H28B C28 H28A 88.8 . . ?
C27 C28 H30C 125.1 . . ?
H28B C28 H30C 89.7 . . ?
H28A C28 H30C 89.5 . . ?

_refine_diff_density_max         0.363
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_2L_3DMF
_database_code_depnum_ccdc_archive 'CCDC 1551278'
_audit_update_record             
;
2017-05-20 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C24 H14 F12 N4 O2), 3(C3 H7 N O)'
_chemical_formula_sum            'C57 H49 F24 N11 O7'
_chemical_formula_weight         1456.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.6244(8)
_cell_length_b                   21.5012(8)
_cell_length_c                   20.8320(9)
_cell_angle_alpha                90
_cell_angle_beta                 111.626(5)
_cell_angle_gamma                90
_cell_volume                     6922.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4874
_cell_measurement_theta_min      3.5250
_cell_measurement_theta_max      22.2760

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_F_000             2960.0
_exptl_transmission_factor_min   0.961
_exptl_transmission_factor_max   0.972
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.137
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36632
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.017
_diffrn_reflns_theta_max         28.957
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             17117
_reflns_number_gt                5729
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1400P)²+0.7936P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17117
_refine_ls_number_parameters     934
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2039
_refine_ls_R_factor_gt           0.1122
_refine_ls_wR_factor_ref         0.3654
_refine_ls_wR_factor_gt          0.3241
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002

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
F2A F 0.5762(7) 0.7420(3) 0.1216(3) 0.119(3) Uani 0.5 1 d . . P A 1
F12A F 1.0111(8) 0.3173(4) 0.6918(5) 0.126(4) Uani 0.5 1 d . . P B 1
F13A F 0.2491(7) 0.6202(5) 0.0443(6) 0.135(4) Uani 0.5 1 d . . P C 1
F21A F 1.0073(13) 0.6688(7) 0.8548(11) 0.183(9) Uani 0.5 1 d . . P D 1
F2B F 0.5453(9) 0.6779(4) 0.0292(3) 0.180(6) Uani 0.5 1 d . . P A 2
F12B F 0.9577(9) 0.3368(6) 0.7114(9) 0.199(7) Uani 0.5 1 d . . P B 2
F13B F 0.3030(11) 0.6281(9) 0.0254(6) 0.203(8) Uani 0.5 1 d . . P C 2
F21B F 1.0383(14) 0.6560(9) 0.8908(9) 0.194(9) Uani 0.5 1 d . . P D 2
O2 O 1.0100(2) 0.51370(15) 0.62283(16) 0.0924(10) Uani 1 1 d . . . . .
O1 O 0.7940(2) 0.68353(15) 0.32593(16) 0.0863(10) Uani 1 1 d . . . . .
F3 F 0.5090(7) 0.7047(7) 0.0634(8) 0.369(9) Uani 1 1 d . . . . .
N1 N 0.7347(2) 0.58693(16) 0.31581(17) 0.0704(9) Uani 1 1 d . . . . .
H1N H 0.7371 0.5536 0.3393 0.084 Uiso 1 1 calc R U . . .
O3 O 0.5551(2) 0.56951(17) 0.36866(17) 0.0961(11) Uani 1 1 d . . . . .
F9 F 1.2721(4) 0.3979(2) 0.98073(19) 0.203(3) Uani 1 1 d . . . . .
O4 O 0.7444(2) 0.41440(18) 0.67816(17) 0.0978(11) Uani 1 1 d . . . . .
N3 N 1.0813(2) 0.60770(18) 0.63420(18) 0.0795(11) Uani 1 1 d . . . . .
H3N H 1.1238 0.6284 0.6626 0.095 Uiso 1 1 calc R U . . .
N2 N 0.8548(2) 0.61041(17) 0.40780(17) 0.0757(10) Uani 1 1 d . . . . .
H2N H 0.8514 0.5714 0.4156 0.091 Uiso 1 1 calc R U . . .
N4 N 1.1321(2) 0.53463(18) 0.71573(18) 0.0815(11) Uani 1 1 d . . . . .
H4N H 1.1749 0.5602 0.7304 0.098 Uiso 1 1 calc R U . . .
O5 O 0.7937(3) 0.48968(17) 0.4222(2) 0.1119(13) Uani 1 1 d . . . . .
F20 F 1.1287(3) 0.6128(2) 0.8799(3) 0.189(2) Uani 1 1 d . . . . .
F8 F 1.2163(3) 0.4811(2) 0.98032(17) 0.1618(17) Uani 1 1 d . . . . .
C9 C 0.7944(3) 0.6320(2) 0.3479(2) 0.0667(11) Uani 1 1 d . . . . .
F24 F 1.0274(3) 0.4195(3) 0.9621(3) 0.228(3) Uani 1 1 d . . . . .
N7 N 0.6994(3) 0.47997(19) 0.58477(19) 0.0900(12) Uani 1 1 d . . . . .
H7N H 0.7095 0.5162 0.5718 0.108 Uiso 1 1 calc R U . . .
C16 C 1.0690(3) 0.5484(2) 0.6542(2) 0.0708(12) Uani 1 1 d . . . . .
N5 N 0.4284(2) 0.55574(19) 0.2759(2) 0.0873(12) Uani 1 1 d . . . . .
H5N H 0.3879 0.5292 0.2569 0.105 Uiso 1 1 calc R U . . .
N8 N 0.8221(3) 0.50252(19) 0.67568(18) 0.0859(12) Uani 1 1 d . . . . .
H8N H 0.8288 0.5291 0.6472 0.103 Uiso 1 1 calc R U . . .
F22 F 0.9246(5) 0.3694(2) 0.8901(2) 0.195(2) Uani 1 1 d . . . . .
N9 N 0.7949(3) 0.40153(19) 0.4805(2) 0.0838(11) Uani 1 1 d . . . . .
N6 N 0.4773(3) 0.4823(2) 0.3601(2) 0.0919(12) Uani 1 1 d . . . . .
H6N H 0.4356 0.4616 0.3307 0.110 Uiso 1 1 calc R U . . .
O6 O 0.3166(2) 0.4497(2) 0.2461(2) 0.1239(14) Uani 1 1 d . . . . .
C17 C 1.1352(3) 0.4829(2) 0.7581(2) 0.0726(12) Uani 1 1 d . . . . .
C7 C 0.6710(3) 0.5883(2) 0.2503(2) 0.0634(10) Uani 1 1 d . . . . .
F15 F 0.2152(3) 0.6947(3) 0.0614(3) 0.221(3) Uani 1 1 d . . . . .
F5 F 0.4230(3) 0.4863(2) 0.1135(3) 0.185(2) Uani 1 1 d . . . . .
C6 C 0.6203(3) 0.5357(2) 0.2277(2) 0.0703(11) Uani 1 1 d . . . . .
H6 H 0.6276 0.5022 0.2575 0.084 Uiso 1 1 calc R U . . .
C12 C 1.0306(3) 0.6387(2) 0.5706(2) 0.0678(11) Uani 1 1 d . . . . .
F1 F 0.6487(4) 0.7065(3) 0.0846(3) 0.229(3) Uani 1 1 d . . . . .
C8 C 0.6574(3) 0.6389(2) 0.2049(2) 0.0705(11) Uani 1 1 d . . . . .
H8 H 0.6906 0.6748 0.2189 0.085 Uiso 1 1 calc R U . . .
C10 C 0.9209(3) 0.64208(19) 0.4580(2) 0.0638(11) Uani 1 1 d . . . . .
C24 C 1.0848(3) 0.4298(2) 0.7355(2) 0.0731(12) Uani 1 1 d . . . . .
H24 H 1.0479 0.4260 0.6896 0.088 Uiso 1 1 calc R U . . .
C11 C 0.9650(3) 0.61028(19) 0.5171(2) 0.0668(11) Uani 1 1 d . . . . .
H11 H 0.9509 0.5691 0.5215 0.080 Uiso 1 1 calc R U . . .
C43 C 0.9946(3) 0.5655(2) 0.8270(2) 0.0753(13) Uani 1 1 d . . . . .
F23 F 0.9015(4) 0.4412(3) 0.9468(2) 0.188(2) Uani 1 1 d . . . . .
O7 O 0.2313(3) 0.4036(2) 0.4303(3) 0.160(2) Uani 1 1 d . . . . .
F10 F 1.0881(4) 0.2763(2) 0.7627(4) 0.210(3) Uani 1 1 d . . . . .
F19 F 1.0543(4) 0.6522(3) 0.7921(3) 0.194(2) Uani 1 1 d . . . . .
F17 F 0.5090(4) 0.7880(2) 0.3244(3) 0.190(2) Uani 1 1 d . . . . .
C18 C 1.1891(3) 0.4868(2) 0.8260(2) 0.0746(12) Uani 1 1 d . . . . .
H18 H 1.2227 0.5223 0.8415 0.090 Uiso 1 1 calc R U . . .
C33 C 0.4931(3) 0.5380(2) 0.3379(2) 0.0792(13) Uani 1 1 d . . . . .
C2 C 0.5946(3) 0.6354(2) 0.1393(2) 0.0761(12) Uani 1 1 d . . . . .
C41 C 0.8814(3) 0.5067(2) 0.7427(2) 0.0723(12) Uani 1 1 d . . . . .
C4 C 0.5591(3) 0.5324(2) 0.1616(2) 0.0781(13) Uani 1 1 d . . . . .
C19 C 1.1948(3) 0.4395(3) 0.8719(2) 0.0831(14) Uani 1 1 d . . . . .
C39 C 0.5906(3) 0.4785(2) 0.4742(2) 0.0792(13) Uani 1 1 d . . . . .
H39 H 0.6137 0.5157 0.4660 0.095 Uiso 1 1 calc R U . . .
C38 C 0.6296(3) 0.4483(2) 0.5380(2) 0.0806(13) Uani 1 1 d . . . . .
C15 C 0.9439(3) 0.7042(2) 0.4504(2) 0.0787(13) Uani 1 1 d . . . . .
H15 H 0.9158 0.7260 0.4097 0.094 Uiso 1 1 calc R U . . .
F18 F 0.5957(3) 0.7619(2) 0.2846(3) 0.194(2) Uani 1 1 d . . . . .
C34 C 0.5176(3) 0.4534(2) 0.4226(2) 0.0810(13) Uani 1 1 d . . . . .
C13 C 1.0544(3) 0.6986(2) 0.5649(2) 0.0814(13) Uani 1 1 d . . . . .
H13 H 1.1000 0.7171 0.6003 0.098 Uiso 1 1 calc R U . . .
C14 C 1.0087(3) 0.7314(2) 0.5047(2) 0.0828(14) Uani 1 1 d . . . . .
H14 H 1.0226 0.7729 0.5012 0.099 Uiso 1 1 calc R U . . .
C42 C 0.9352(3) 0.5584(2) 0.7594(2) 0.0713(11) Uani 1 1 d . . . . .
H42 H 0.9317 0.5881 0.7260 0.086 Uiso 1 1 calc R U . . .
C48 C 0.8882(3) 0.4632(2) 0.7933(2) 0.0784(13) Uani 1 1 d . . . . .
H48 H 0.8524 0.4284 0.7829 0.094 Uiso 1 1 calc R U . . .
C3 C 0.5443(3) 0.5833(3) 0.1177(2) 0.0830(14) Uani 1 1 d . . . . .
H3 H 0.5007 0.5820 0.0741 0.100 Uiso 1 1 calc R U . . .
F11 F 1.0047(5) 0.3056(3) 0.7987(3) 0.223(3) Uani 1 1 d . . . . .
C40 C 0.7534(3) 0.4616(3) 0.6477(3) 0.0838(14) Uani 1 1 d . . . . .
C22 C 1.0902(3) 0.3832(2) 0.7818(2) 0.0792(13) Uani 1 1 d . . . . .
F14 F 0.3071(4) 0.7132(3) 0.0273(2) 0.205(2) Uani 1 1 d . . . . .
F4 F 0.5189(4) 0.4484(2) 0.0895(4) 0.230(3) Uani 1 1 d . . . . .
C31 C 0.4229(3) 0.6116(2) 0.2419(2) 0.0793(13) Uani 1 1 d . . . . .
C45 C 1.0003(3) 0.5227(3) 0.8753(2) 0.0841(14) Uani 1 1 d . . . . .
H45 H 1.0400 0.5279 0.9201 0.101 Uiso 1 1 calc R U . . .
C46 C 0.9480(3) 0.4714(3) 0.8589(2) 0.0832(14) Uani 1 1 d . . . . .
C32 C 0.3618(3) 0.6161(2) 0.1753(3) 0.0834(13) Uani 1 1 d . . . . .
H32 H 0.3266 0.5821 0.1560 0.100 Uiso 1 1 calc R U . . .
C37 C 0.5966(4) 0.3935(2) 0.5500(3) 0.0931(15) Uani 1 1 d . . . . .
H37 H 0.6220 0.3734 0.5922 0.112 Uiso 1 1 calc R U . . .
N11 N 0.2498(4) 0.3140(3) 0.4856(3) 0.1209(17) Uani 1 1 d . . . . .
C26 C 0.3523(3) 0.6697(3) 0.1373(3) 0.0907(15) Uani 1 1 d . . . . .
C35 C 0.4889(4) 0.3964(2) 0.4370(3) 0.0951(16) Uani 1 1 d . . . . .
H35 H 0.4429 0.3773 0.4026 0.114 Uiso 1 1 calc R U . . .
C1 C 0.5820(4) 0.6885(4) 0.0933(3) 0.105(2) Uani 1 1 d . . . . .
C30 C 0.4723(3) 0.6641(3) 0.2698(3) 0.0886(15) Uani 1 1 d . . . . .
H30 H 0.5130 0.6626 0.3147 0.106 Uiso 1 1 calc R U . . .
C21 C 1.1451(4) 0.3881(3) 0.8502(2) 0.0890(15) Uani 1 1 d . . . . .
H21 H 1.1479 0.3562 0.8811 0.107 Uiso 1 1 calc R U . . .
C28 C 0.4622(4) 0.7182(2) 0.2327(3) 0.0859(14) Uani 1 1 d . . . . .
N10 N 0.2366(4) 0.3774(3) 0.1897(4) 0.133(2) Uani 1 1 d . . . . .
C27 C 0.4014(3) 0.7210(3) 0.1672(3) 0.0931(15) Uani 1 1 d . . . . .
H27 H 0.3930 0.7581 0.1425 0.112 Uiso 1 1 calc R U . . .
C51 C 0.8211(4) 0.4571(3) 0.4742(3) 0.0977(16) Uani 1 1 d . . . . .
H51 H 0.8645 0.4739 0.5125 0.117 Uiso 1 1 calc R U . . .
C20 C 1.2525(5) 0.4480(3) 0.9455(3) 0.1050(18) Uani 1 1 d . . . . .
F7 F 1.3238(3) 0.4749(3) 0.95501(18) 0.192(3) Uani 1 1 d . . . . .
C44 C 1.0475(4) 0.6213(3) 0.8451(3) 0.0980(16) Uani 1 1 d . . . . .
C23 C 1.0356(6) 0.3261(3) 0.7563(4) 0.113(2) Uani 1 1 d . . . . .
C36 C 0.5244(4) 0.3674(3) 0.4985(3) 0.114(2) Uani 1 1 d . . . . .
H36 H 0.5010 0.3303 0.5066 0.136 Uiso 1 1 calc R U . . .
C5 C 0.5050(5) 0.4766(3) 0.1381(3) 0.115(2) Uani 1 1 d . . . . .
C57 C 0.2570(7) 0.3694(5) 0.4781(5) 0.172(4) Uani 1 1 d . . . . .
H57 H 0.2901 0.3894 0.5188 0.207 Uiso 1 1 calc R U . . .
C50 C 0.7258(4) 0.3738(3) 0.4229(3) 0.1160(19) Uani 1 1 d . . . . .
H50A H 0.7095 0.4016 0.3841 0.174 Uiso 1 1 calc R U . . .
H50B H 0.6768 0.3664 0.4358 0.174 Uiso 1 1 calc R U . . .
H50C H 0.7453 0.3352 0.4107 0.174 Uiso 1 1 calc R U . . .
F16 F 0.5000(4) 0.8204(2) 0.2292(3) 0.229(3) Uani 1 1 d . . . . .
C47 C 0.9524(5) 0.4239(4) 0.9134(3) 0.126(2) Uani 1 1 d . . . . .
C29 C 0.5130(5) 0.7720(3) 0.2638(4) 0.115(2) Uani 1 1 d . . . . .
C49 C 0.8319(5) 0.3675(3) 0.5437(4) 0.141(3) Uani 1 1 d . . . . .
H49A H 0.8754 0.3924 0.5770 0.211 Uiso 1 1 calc R U . . .
H49B H 0.8576 0.3299 0.5353 0.211 Uiso 1 1 calc R U . . .
H49C H 0.7875 0.3574 0.5611 0.211 Uiso 1 1 calc R U . . .
C56 C 0.1822(5) 0.2852(4) 0.4291(5) 0.163(3) Uani 1 1 d . . . . .
H56A H 0.1483 0.3168 0.3983 0.245 Uiso 1 1 calc R U . . .
H56B H 0.1458 0.2613 0.4465 0.245 Uiso 1 1 calc R U . . .
H56C H 0.2072 0.2584 0.4047 0.245 Uiso 1 1 calc R U . . .
F6 F 0.5099(4) 0.4385(2) 0.1851(3) 0.259(4) Uani 1 1 d . . . . .
C53 C 0.1873(7) 0.3487(5) 0.1210(6) 0.239(6) Uani 1 1 d . . . . .
H53A H 0.2052 0.3673 0.0865 0.359 Uiso 1 1 calc R U . . .
H53B H 0.1265 0.3556 0.1093 0.359 Uiso 1 1 calc R U . . .
H53C H 0.1986 0.3048 0.1230 0.359 Uiso 1 1 calc R U . . .
C55 C 0.3025(8) 0.2823(5) 0.5491(6) 0.216(5) Uani 1 1 d . . . . .
H55A H 0.3545 0.3056 0.5718 0.324 Uiso 1 1 calc R U . . .
H55B H 0.3171 0.2414 0.5382 0.324 Uiso 1 1 calc R U . . .
H55C H 0.2706 0.2789 0.5791 0.324 Uiso 1 1 calc R U . . .
C25 C 0.2883(5) 0.6698(4) 0.0637(4) 0.119(2) Uani 1 1 d . . . . .
C54 C 0.2806(5) 0.4131(6) 0.1960(4) 0.198(5) Uani 1 1 d . . . . .
H54 H 0.2965 0.4195 0.1581 0.238 Uiso 1 1 calc R U . . .
C52 C 0.2419(6) 0.3368(4) 0.2465(5) 0.182(4) Uani 1 1 d . . . . .
H52A H 0.2922 0.3109 0.2577 0.273 Uiso 1 1 calc R U . . .
H52B H 0.1910 0.3112 0.2335 0.273 Uiso 1 1 calc R U . . .
H52C H 0.2458 0.3614 0.2860 0.273 Uiso 1 1 calc R U . . .


_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
F2A C1 1.312(9) . ?
F2A F3 1.536(16) . ?
F12A C23 1.267(11) . ?
F13A C25 1.239(12) . ?
F13A F15 1.778(14) . ?
F21A C44 1.276(15) . ?
F2B F3 1.234(16) . ?
F2B C1 1.268(9) . ?
F12B C23 1.308(12) . ?
F13B C25 1.283(13) . ?
F21B C44 1.262(15) . ?
O2 C16 1.214(5) . ?
O1 C9 1.198(5) . ?
F3 C1 1.194(9) . ?
N1 C9 1.371(5) . ?
N1 C7 1.386(5) . ?
O3 C33 1.203(5) . ?
F9 C20 1.276(7) . ?
O4 C40 1.235(6) . ?
N3 C16 1.381(6) . ?
N3 C12 1.444(5) . ?
N2 C9 1.363(5) . ?
N2 C10 1.385(5) . ?
N4 C16 1.356(5) . ?
N4 C17 1.409(5) . ?
O5 C51 1.228(6) . ?
F20 C44 1.288(6) . ?
F8 C20 1.312(7) . ?
F24 C47 1.289(8) . ?
N7 C40 1.347(6) . ?
N7 C38 1.387(6) . ?
N5 C31 1.379(6) . ?
N5 C33 1.396(6) . ?
N8 C41 1.384(5) . ?
N8 C40 1.388(6) . ?
F22 C47 1.287(8) . ?
N9 C51 1.295(6) . ?
N9 C49 1.431(7) . ?
N9 C50 1.449(7) . ?
N6 C33 1.343(6) . ?
N6 C34 1.374(6) . ?
O6 C54 1.268(9) . ?
C17 C18 1.370(6) . ?
C17 C24 1.392(6) . ?
C7 C6 1.385(6) . ?
C7 C8 1.405(6) . ?
F15 C25 1.314(9) . ?
F5 C5 1.285(8) . ?
C6 C4 1.380(6) . ?
C12 C13 1.367(6) . ?
C12 C11 1.381(6) . ?
F1 C1 1.251(7) . ?
C8 C2 1.382(6) . ?
C10 C11 1.362(5) . ?
C10 C15 1.413(6) . ?
C24 C22 1.372(6) . ?
C43 C45 1.341(7) . ?
C43 C42 1.398(6) . ?
C43 C44 1.453(8) . ?
F23 C47 1.333(8) . ?
O7 C57 1.183(8) . ?
F10 C23 1.358(9) . ?
F19 C44 1.330(7) . ?
F17 C29 1.333(8) . ?
C18 C19 1.376(6) . ?
C2 C3 1.371(7) . ?
C2 C1 1.456(7) . ?
C41 C48 1.383(6) . ?
C41 C42 1.388(6) . ?
C4 C3 1.387(7) . ?
C4 C5 1.471(8) . ?
C19 C21 1.353(7) . ?
C19 C20 1.489(7) . ?
C39 C34 1.399(6) . ?
C39 C38 1.406(6) . ?
C38 C37 1.361(7) . ?
C15 C14 1.373(6) . ?
F18 C29 1.298(7) . ?
C34 C35 1.388(7) . ?
C13 C14 1.395(6) . ?
C48 C46 1.374(6) . ?
F11 C23 1.254(7) . ?
C22 C21 1.384(6) . ?
C22 C23 1.502(8) . ?
F14 C25 1.311(9) . ?
F4 C5 1.273(8) . ?
C31 C32 1.388(6) . ?
C31 C30 1.392(7) . ?
C45 C46 1.366(7) . ?
C46 C47 1.509(8) . ?
C32 C26 1.374(7) . ?
C37 C36 1.399(7) . ?
N11 C57 1.213(9) . ?
N11 C56 1.434(9) . ?
N11 C55 1.459(10) . ?
C26 C27 1.378(7) . ?
C26 C25 1.510(8) . ?
C35 C36 1.348(7) . ?
C30 C28 1.373(7) . ?
C28 C27 1.368(7) . ?
C28 C29 1.436(8) . ?
N10 C54 1.035(9) . ?
N10 C52 1.447(9) . ?
N10 C53 1.496(11) . ?
C20 F7 1.268(7) . ?
C5 F6 1.255(7) . ?
F16 C29 1.239(7) . ?

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
C1 F2A F3 48.8(5) . . ?
C25 F13A F15 47.6(6) . . ?
F3 F2B C1 57.0(6) . . ?
C1 F3 F2B 62.9(8) . . ?
C1 F3 F2A 55.7(7) . . ?
C9 N1 C7 128.2(3) . . ?
C16 N3 C12 127.0(4) . . ?
C9 N2 C10 129.5(4) . . ?
C16 N4 C17 126.9(4) . . ?
O1 C9 N2 124.3(4) . . ?
O1 C9 N1 124.5(4) . . ?
N2 C9 N1 111.3(4) . . ?
C40 N7 C38 128.7(4) . . ?
O2 C16 N4 124.5(4) . . ?
O2 C16 N3 125.8(4) . . ?
N4 C16 N3 109.7(4) . . ?
C31 N5 C33 126.6(4) . . ?
C41 N8 C40 129.4(4) . . ?
C51 N9 C49 121.3(5) . . ?
C51 N9 C50 119.2(5) . . ?
C49 N9 C50 119.5(5) . . ?
C33 N6 C34 129.8(4) . . ?
C18 C17 C24 118.9(4) . . ?
C18 C17 N4 117.2(4) . . ?
C24 C17 N4 123.8(4) . . ?
C6 C7 N1 117.8(4) . . ?
C6 C7 C8 118.4(4) . . ?
N1 C7 C8 123.7(4) . . ?
C25 F15 F13A 44.1(5) . . ?
C4 C6 C7 121.0(4) . . ?
C13 C12 C11 120.9(4) . . ?
C13 C12 N3 115.2(4) . . ?
C11 C12 N3 123.8(4) . . ?
C2 C8 C7 119.9(4) . . ?
C11 C10 N2 116.7(4) . . ?
C11 C10 C15 119.9(4) . . ?
N2 C10 C15 123.5(4) . . ?
C22 C24 C17 119.1(4) . . ?
C10 C11 C12 120.6(4) . . ?
C45 C43 C42 120.6(5) . . ?
C45 C43 C44 120.2(4) . . ?
C42 C43 C44 119.1(5) . . ?
C17 C18 C19 121.5(5) . . ?
O3 C33 N6 123.9(5) . . ?
O3 C33 N5 123.7(5) . . ?
N6 C33 N5 112.4(4) . . ?
C3 C2 C8 121.1(4) . . ?
C3 C2 C1 120.2(5) . . ?
C8 C2 C1 118.7(5) . . ?
C48 C41 N8 123.5(4) . . ?
C48 C41 C42 119.1(4) . . ?
N8 C41 C42 117.3(4) . . ?
C6 C4 C3 120.2(4) . . ?
C6 C4 C5 120.6(5) . . ?
C3 C4 C5 119.0(4) . . ?
C21 C19 C18 119.7(4) . . ?
C21 C19 C20 121.8(5) . . ?
C18 C19 C20 118.5(5) . . ?
C34 C39 C38 121.0(5) . . ?
C37 C38 N7 125.9(5) . . ?
C37 C38 C39 119.7(4) . . ?
N7 C38 C39 114.4(4) . . ?
C14 C15 C10 118.3(4) . . ?
N6 C34 C35 121.2(5) . . ?
N6 C34 C39 122.4(5) . . ?
C35 C34 C39 116.4(5) . . ?
C12 C13 C14 118.4(4) . . ?
C15 C14 C13 121.8(4) . . ?
C41 C42 C43 119.3(4) . . ?
C46 C48 C41 119.8(5) . . ?
C2 C3 C4 119.3(4) . . ?
O4 C40 N7 125.3(5) . . ?
O4 C40 N8 122.8(5) . . ?
N7 C40 N8 111.9(5) . . ?
C24 C22 C21 121.1(5) . . ?
C24 C22 C23 118.3(5) . . ?
C21 C22 C23 120.7(5) . . ?
N5 C31 C32 117.3(4) . . ?
N5 C31 C30 125.1(4) . . ?
C32 C31 C30 117.6(5) . . ?
C43 C45 C46 120.3(4) . . ?
C45 C46 C48 120.8(5) . . ?
C45 C46 C47 120.6(5) . . ?
C48 C46 C47 118.5(6) . . ?
C26 C32 C31 121.4(5) . . ?
C38 C37 C36 119.8(5) . . ?
C57 N11 C56 113.7(8) . . ?
C57 N11 C55 121.4(8) . . ?
C56 N11 C55 124.7(8) . . ?
C32 C26 C27 119.3(5) . . ?
C32 C26 C25 118.4(5) . . ?
C27 C26 C25 122.3(6) . . ?
C36 C35 C34 123.3(5) . . ?
F3 C1 F1 128.2(7) . . ?
F3 C1 F2B 60.1(9) . . ?
F1 C1 F2B 90.6(8) . . ?
F3 C1 F2A 75.5(10) . . ?
F1 C1 F2A 90.5(7) . . ?
F3 C1 C2 116.4(7) . . ?
F1 C1 C2 114.8(5) . . ?
F2B C1 C2 116.7(7) . . ?
F2A C1 C2 114.2(5) . . ?
C28 C30 C31 121.4(5) . . ?
C19 C21 C22 119.7(5) . . ?
C27 C28 C30 119.4(5) . . ?
C27 C28 C29 120.7(6) . . ?
C30 C28 C29 119.8(6) . . ?
C54 N10 C52 121.3(10) . . ?
C54 N10 C53 122.6(9) . . ?
C52 N10 C53 112.4(8) . . ?
C28 C27 C26 120.8(5) . . ?
O5 C51 N9 126.0(6) . . ?
F7 C20 F9 105.6(6) . . ?
F7 C20 F8 105.0(6) . . ?
F9 C20 F8 102.2(5) . . ?
F7 C20 C19 115.4(5) . . ?
F9 C20 C19 114.8(6) . . ?
F8 C20 C19 112.5(5) . . ?
F21B C44 F20 93.0(11) . . ?
F21A C44 F20 121.6(10) . . ?
F21B C44 F19 113.7(11) . . ?
F21A C44 F19 86.6(11) . . ?
F20 C44 F19 98.4(6) . . ?
F21B C44 C43 117.1(12) . . ?
F21A C44 C43 113.6(11) . . ?
F20 C44 C43 116.0(5) . . ?
F19 C44 C43 115.2(5) . . ?
F11 C23 F12A 129.7(8) . . ?
F11 C23 F12B 90.7(11) . . ?
F11 C23 F10 93.9(6) . . ?
F12A C23 F10 85.9(8) . . ?
F12B C23 F10 129.8(9) . . ?
F11 C23 C22 113.0(6) . . ?
F12A C23 C22 114.4(6) . . ?
F12B C23 C22 114.9(7) . . ?
F10 C23 C22 109.0(7) . . ?
C35 C36 C37 119.6(5) . . ?
F6 C5 F4 109.3(7) . . ?
F6 C5 F5 99.9(8) . . ?
F4 C5 F5 103.8(6) . . ?
F6 C5 C4 114.7(5) . . ?
F4 C5 C4 112.6(7) . . ?
F5 C5 C4 115.4(6) . . ?
O7 C57 N11 134.2(11) . . ?
F22 C47 F24 109.9(8) . . ?
F22 C47 F23 104.0(7) . . ?
F24 C47 F23 102.9(6) . . ?
F22 C47 C46 115.0(6) . . ?
F24 C47 C46 113.9(7) . . ?
F23 C47 C46 109.8(7) . . ?
F16 C29 F18 105.7(7) . . ?
F16 C29 F17 106.0(6) . . ?
F18 C29 F17 98.2(7) . . ?
F16 C29 C28 117.8(7) . . ?
F18 C29 C28 113.0(5) . . ?
F17 C29 C28 114.1(6) . . ?
F13A C25 F14 129.3(9) . . ?
F13B C25 F14 89.9(12) . . ?
F13A C25 F15 88.2(9) . . ?
F13B C25 F15 130.4(11) . . ?
F14 C25 F15 96.0(6) . . ?
F13A C25 C26 114.8(8) . . ?
F13B C25 C26 114.0(8) . . ?
F14 C25 C26 111.1(7) . . ?
F15 C25 C26 109.5(7) . . ?
N10 C54 O6 131.3(9) . . ?

_refine_diff_density_max         0.581
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_L_2DMSO
_database_code_depnum_ccdc_archive 'CCDC 1551279'
_audit_update_record             
;
2017-05-20 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H14 F12 N4 O2, 2(C2 H6 O S)'
_chemical_formula_sum            'C28 H26 F12 N4 O4 S2'
_chemical_formula_weight         774.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.9692(15)
_cell_length_b                   20.9828(14)
_cell_length_c                   9.5322(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.706(9)
_cell_angle_gamma                90
_cell_volume                     3476.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2638
_cell_measurement_theta_min      3.6360
_cell_measurement_theta_max      22.1500

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             1576.0
_exptl_transmission_factor_min   0.929
_exptl_transmission_factor_max   0.955
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.256
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17317
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.941
_diffrn_reflns_theta_max         28.827
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8651
_reflns_number_gt                3326
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1100P)²+0.7161P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8651
_refine_ls_number_parameters     519
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1866
_refine_ls_R_factor_gt           0.0957
_refine_ls_wR_factor_ref         0.3055
_refine_ls_wR_factor_gt          0.2466
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002

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
S1A S 0.8563(3) 0.6992(3) 0.3584(8) 0.190(2) Uani 0.5 1 d . . P A 1
S2A S 0.44917(19) 0.57333(17) 0.9323(3) 0.0684(7) Uani 0.5 1 d . . P B 1
F1A F 0.8118(10) 1.2080(4) 0.303(2) 0.217(7) Uani 0.5 1 d . . P C 1
F5A F 0.9515(5) 0.9860(6) 0.1153(7) 0.151(4) Uani 0.5 1 d . . P D 1
F7A F 0.5754(8) 0.3294(8) 0.5548(14) 0.147(4) Uani 0.5 1 d . . P E 1
F8A F 0.6295(14) 0.3110(5) 0.654(3) 0.190(9) Uani 0.5 1 d . . P E 1
F10A F 0.8702(13) 0.4269(9) 0.356(3) 0.260(13) Uani 0.5 1 d . . P F 1
S1B S 0.89317(16) 0.70089(14) 0.4681(3) 0.0771(7) Uani 0.5 1 d . . P A 2
S2B S 0.4247(6) 0.5754(4) 0.8644(14) 0.324(7) Uani 0.5 1 d . . P B 2
F1B F 0.8157(7) 1.2087(3) 0.4492(15) 0.134(3) Uani 0.5 1 d . . P C 2
F5B F 0.9876(4) 0.9195(3) 0.3227(8) 0.114(3) Uani 0.5 1 d . . P D 2
F7B F 0.6430(9) 0.3465(13) 0.770(2) 0.200(9) Uani 0.5 1 d . . P E 2
F8B F 0.6122(11) 0.3905(6) 0.7754(16) 0.145(5) Uani 0.5 1 d . . P E 2
F10B F 0.8389(10) 0.4255(8) 0.2883(13) 0.130(5) Uani 0.5 1 d . . P F 2
N4 N 0.7158(2) 0.57913(17) 0.5454(5) 0.0893(12) Uani 1 1 d . . . . .
H4N H 0.7495 0.5972 0.5087 0.107 Uiso 1 1 calc R U . . .
O1 O 0.78325(19) 0.88078(15) 0.4988(4) 0.1109(12) Uani 1 1 d . . . . .
O4 O 0.3731(2) 0.54078(17) 0.8992(5) 0.1258(14) Uani 1 1 d . . . . .
O2 O 0.62311(19) 0.60164(15) 0.6641(4) 0.1100(12) Uani 1 1 d . . . . .
C25 C 0.8155(2) 0.6707(2) 0.4551(6) 0.0844(14) Uani 1 1 d . . . . .
H25C H 0.7806 0.7013 0.4778 0.127 Uiso 1 1 calc R U . A 1
H25B H 0.8516 0.6575 0.5427 0.127 Uiso 1 1 calc R U . A 1
H25A H 0.7871 0.6344 0.4088 0.127 Uiso 1 1 calc R U . A 1
N1 N 0.7477(2) 0.98497(17) 0.4932(4) 0.0894(12) Uani 1 1 d . . . . .
H1N H 0.7136 1.0102 0.5113 0.107 Uiso 1 1 calc R U . . .
N3 N 0.6890(2) 0.68187(17) 0.5883(4) 0.0867(12) Uani 1 1 d . . . . .
H3N H 0.7255 0.6884 0.5466 0.104 Uiso 1 1 calc R U . . .
N2 N 0.6806(2) 0.91066(17) 0.5835(4) 0.0857(11) Uani 1 1 d . . . . .
H2N H 0.6550 0.9436 0.5980 0.103 Uiso 1 1 calc R U . . .
F11 F 0.7826(3) 0.3459(2) 0.2807(5) 0.1646(16) Uani 1 1 d . . . . .
C16 C 0.6718(2) 0.6200(2) 0.6046(5) 0.0783(12) Uani 1 1 d . . . . .
C14 C 0.6557(2) 0.7369(2) 0.6298(5) 0.0702(11) Uani 1 1 d . . . . .
C10 C 0.6559(2) 0.8516(2) 0.6255(5) 0.0717(11) Uani 1 1 d . . . . .
C9 C 0.7401(3) 0.9219(2) 0.5228(5) 0.0821(13) Uani 1 1 d . . . . .
C15 C 0.6818(2) 0.7936(2) 0.5853(5) 0.0739(12) Uani 1 1 d . . . . .
H15 H 0.7168 0.7929 0.5284 0.089 Uiso 1 1 calc R U . . .
C7 C 0.8041(2) 1.0132(2) 0.4372(5) 0.0756(12) Uani 1 1 d . . . . .
C11 C 0.6022(2) 0.8518(2) 0.7076(5) 0.0843(13) Uani 1 1 d . . . . .
H11 H 0.5836 0.8900 0.7346 0.101 Uiso 1 1 calc R U . . .
C24 C 0.7622(2) 0.4841(2) 0.4663(5) 0.0778(12) Uani 1 1 d . . . . .
H24 H 0.7943 0.5088 0.4256 0.093 Uiso 1 1 calc R U . . .
F4 F 1.0277(3) 0.9984(3) 0.2743(7) 0.208(2) Uani 1 1 d . . . . .
C22 C 0.7642(3) 0.4190(2) 0.4552(5) 0.0823(13) Uani 1 1 d . . . . .
C17 C 0.7135(2) 0.5136(2) 0.5368(5) 0.0728(11) Uani 1 1 d . . . . .
F12 F 0.8690(3) 0.3527(3) 0.4665(5) 0.1736(18) Uani 1 1 d . . . . .
C4 C 0.9084(3) 1.0112(2) 0.3215(5) 0.0856(13) Uani 1 1 d . . . . .
C6 C 0.8540(2) 0.9788(2) 0.3744(5) 0.0777(12) Uani 1 1 d . . . . .
H6 H 0.8506 0.9346 0.3681 0.093 Uiso 1 1 calc R U . . .
C12 C 0.5767(3) 0.7945(2) 0.7484(6) 0.0939(15) Uani 1 1 d . . . . .
H12 H 0.5406 0.7949 0.8031 0.113 Uiso 1 1 calc R U . . .
C13 C 0.6023(2) 0.7369(2) 0.7120(5) 0.0852(13) Uani 1 1 d . . . . .
H13 H 0.5843 0.6989 0.7417 0.102 Uiso 1 1 calc R U . . .
C8 C 0.8108(3) 1.0785(2) 0.4437(5) 0.0840(13) Uani 1 1 d . . . . .
H8 H 0.7780 1.1019 0.4854 0.101 Uiso 1 1 calc R U . . .
C19 C 0.6676(3) 0.4108(2) 0.5857(5) 0.0874(14) Uani 1 1 d . . . . .
C21 C 0.7163(3) 0.3804(2) 0.5167(5) 0.0940(15) Uani 1 1 d . . . . .
H21 H 0.7177 0.3362 0.5108 0.113 Uiso 1 1 calc R U . . .
C27 C 0.4290(4) 0.6543(3) 0.8883(8) 0.144(2) Uani 1 1 d . . . . .
H27A H 0.3816 0.6660 0.9107 0.217 Uiso 1 1 calc R U . B 1
H27B H 0.4243 0.6607 0.7867 0.217 Uiso 1 1 calc R U . B 1
H27C H 0.4700 0.6803 0.9436 0.217 Uiso 1 1 calc R U . B 1
C28 C 0.4871(4) 0.5532(4) 0.7848(8) 0.151(3) Uani 1 1 d . . . . .
H28C H 0.5339 0.5764 0.7917 0.227 Uiso 1 1 calc R U . B 1
H28B H 0.4505 0.5639 0.6957 0.227 Uiso 1 1 calc R U . B 1
H28A H 0.4975 0.5083 0.7867 0.227 Uiso 1 1 calc R U . B 1
C5 C 0.9628(4) 0.9743(3) 0.2583(8) 0.117(2) Uani 1 1 d . . . . .
C23 C 0.8163(4) 0.3885(3) 0.3768(9) 0.1137(19) Uani 1 1 d . . . . .
C2 C 0.8642(3) 1.1098(2) 0.3906(6) 0.0939(15) Uani 1 1 d . . . . .
C3 C 0.9138(3) 1.0763(2) 0.3280(5) 0.0935(15) Uani 1 1 d . . . . .
H3 H 0.9501 1.0976 0.2910 0.112 Uiso 1 1 calc R U . . .
F6 F 0.9327(5) 0.9360(7) 0.1764(17) 0.399(9) Uani 1 1 d . . . . .
C18 C 0.6650(3) 0.4760(2) 0.5975(5) 0.0812(12) Uani 1 1 d . . . . .
H18 H 0.6315 0.4949 0.6451 0.097 Uiso 1 1 calc R U . . .
C1 C 0.8661(6) 1.1805(3) 0.3967(12) 0.132(3) Uani 1 1 d . . . . .
F3 F 0.9091(7) 1.1995(3) 0.5197(10) 0.275(4) Uani 1 1 d . . . . .
F2 F 0.9069(8) 1.2069(3) 0.3271(13) 0.299(5) Uani 1 1 d . . . . .
C20 C 0.6159(4) 0.3700(3) 0.6499(10) 0.111(2) Uani 1 1 d . . . . .
O3 O 0.8725(5) 0.7703(4) 0.3568(10) 0.263(4) Uani 1 1 d . . . . .
C26 C 0.9329(4) 0.6549(3) 0.3517(10) 0.184(4) Uani 1 1 d . . . . .
H26B H 0.9690 0.6549 0.4452 0.276 Uiso 1 1 calc R U . A 1
H26C H 0.9569 0.6724 0.2810 0.276 Uiso 1 1 calc R U . A 1
H26A H 0.9167 0.6120 0.3252 0.276 Uiso 1 1 calc R U . A 1
F9 F 0.5472(4) 0.3925(5) 0.6216(16) 0.262(4) 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
S1A C25 1.446(7) . ?
S1A O3 1.521(8) . ?
S1A C26 1.675(8) . ?
S2A O4 1.488(5) . ?
S2A C28 1.762(8) . ?
S2A C27 1.766(7) . ?
F1A C1 1.281(12) . ?
F5A C5 1.349(9) . ?
F7A C20 1.320(12) . ?
F8A C20 1.260(12) . ?
F10A C23 1.315(19) . ?
S1B C25 1.510(5) . ?
S1B C26 1.754(8) . ?
S1B O3 1.785(8) . ?
S2B O4 1.286(7) . ?
S2B C28 1.574(10) . ?
S2B C27 1.671(9) . ?
F1B C1 1.286(10) . ?
F5B C5 1.326(8) . ?
F7B C20 1.230(13) . ?
F8B C20 1.289(13) . ?
F10B C23 1.287(14) . ?
N4 C17 1.377(5) . ?
N4 C16 1.381(5) . ?
O1 C9 1.219(5) . ?
O2 C16 1.220(5) . ?
N1 C9 1.368(5) . ?
N1 C7 1.392(5) . ?
N3 C16 1.353(5) . ?
N3 C14 1.403(5) . ?
N2 C9 1.361(6) . ?
N2 C10 1.407(5) . ?
F11 C23 1.312(7) . ?
C14 C15 1.384(5) . ?
C14 C13 1.384(6) . ?
C10 C11 1.388(6) . ?
C10 C15 1.392(6) . ?
C7 C8 1.375(6) . ?
C7 C6 1.399(5) . ?
C11 C12 1.377(6) . ?
C24 C22 1.371(6) . ?
C24 C17 1.378(5) . ?
F4 C5 1.244(6) . ?
C22 C21 1.413(6) . ?
C22 C23 1.482(7) . ?
C17 C18 1.405(5) . ?
F12 C23 1.334(7) . ?
C4 C3 1.370(6) . ?
C4 C6 1.387(6) . ?
C4 C5 1.488(7) . ?
C12 C13 1.368(6) . ?
C8 C2 1.362(6) . ?
C19 C18 1.373(6) . ?
C19 C21 1.378(6) . ?
C19 C20 1.502(7) . ?
C5 F6 1.155(9) . ?
C2 C3 1.384(7) . ?
C2 C1 1.486(8) . ?
C1 F2 1.237(8) . ?
C1 F3 1.292(10) . ?
C20 F9 1.284(8) . ?

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
C25 S1A O3 122.8(5) . . ?
C25 S1A C26 110.4(5) . . ?
O3 S1A C26 112.6(5) . . ?
O4 S2A C28 104.0(3) . . ?
O4 S2A C27 105.6(3) . . ?
C28 S2A C27 98.0(4) . . ?
C25 S1B C26 103.5(4) . . ?
C25 S1B O3 104.2(4) . . ?
C26 S1B O3 97.5(4) . . ?
O4 S2B C28 127.2(7) . . ?
O4 S2B C27 122.4(6) . . ?
C28 S2B C27 110.2(5) . . ?
C17 N4 C16 129.2(4) . . ?
C9 N1 C7 127.7(4) . . ?
C16 N3 C14 129.1(4) . . ?
C9 N2 C10 127.7(4) . . ?
O2 C16 N3 124.6(4) . . ?
O2 C16 N4 123.2(4) . . ?
N3 C16 N4 112.2(4) . . ?
C15 C14 C13 120.7(4) . . ?
C15 C14 N3 114.7(4) . . ?
C13 C14 N3 124.6(4) . . ?
C11 C10 C15 119.1(4) . . ?
C11 C10 N2 118.2(4) . . ?
C15 C10 N2 122.7(4) . . ?
O1 C9 N2 124.3(4) . . ?
O1 C9 N1 123.0(4) . . ?
N2 C9 N1 112.7(4) . . ?
C14 C15 C10 120.3(4) . . ?
C8 C7 N1 118.1(4) . . ?
C8 C7 C6 118.4(4) . . ?
N1 C7 C6 123.5(4) . . ?
C12 C11 C10 119.0(4) . . ?
C22 C24 C17 121.2(4) . . ?
C24 C22 C21 120.5(4) . . ?
C24 C22 C23 120.2(4) . . ?
C21 C22 C23 119.4(5) . . ?
N4 C17 C24 117.6(4) . . ?
N4 C17 C18 123.3(4) . . ?
C24 C17 C18 119.0(4) . . ?
C3 C4 C6 121.4(4) . . ?
C3 C4 C5 119.3(5) . . ?
C6 C4 C5 119.3(5) . . ?
C4 C6 C7 119.3(4) . . ?
C13 C12 C11 122.8(4) . . ?
C12 C13 C14 118.0(4) . . ?
C2 C8 C7 121.6(4) . . ?
C18 C19 C21 122.6(4) . . ?
C18 C19 C20 119.8(5) . . ?
C21 C19 C20 117.7(5) . . ?
C19 C21 C22 117.5(4) . . ?
F6 C5 F4 129.0(7) . . ?
F6 C5 F5B 75.8(10) . . ?
F4 C5 F5B 95.8(8) . . ?
F6 C5 F5A 61.2(10) . . ?
F4 C5 F5A 86.9(7) . . ?
F6 C5 C4 113.0(7) . . ?
F4 C5 C4 115.6(5) . . ?
F5B C5 C4 116.2(6) . . ?
F5A C5 C4 111.7(7) . . ?
F10B C23 F11 96.9(10) . . ?
F11 C23 F10A 122.5(11) . . ?
F10B C23 F12 117.9(10) . . ?
F11 C23 F12 101.0(5) . . ?
F10A C23 F12 90.8(12) . . ?
F10B C23 C22 114.5(9) . . ?
F11 C23 C22 114.1(5) . . ?
F10A C23 C22 113.3(9) . . ?
F12 C23 C22 110.9(6) . . ?
C8 C2 C3 120.6(5) . . ?
C8 C2 C1 118.5(5) . . ?
C3 C2 C1 120.9(5) . . ?
C4 C3 C2 118.6(4) . . ?
C19 C18 C17 119.2(4) . . ?
F2 C1 F1A 82.8(11) . . ?
F2 C1 F1B 125.2(8) . . ?
F2 C1 F3 92.9(9) . . ?
F1A C1 F3 131.9(10) . . ?
F1B C1 F3 79.8(9) . . ?
F2 C1 C2 115.9(7) . . ?
F1A C1 C2 114.7(8) . . ?
F1B C1 C2 117.6(6) . . ?
F3 C1 C2 110.2(8) . . ?
F7B C20 F9 118.4(12) . . ?
F8A C20 F9 122.3(12) . . ?
F7B C20 F8B 50.9(12) . . ?
F9 C20 F8B 78.4(9) . . ?
F8A C20 F7A 57.1(11) . . ?
F9 C20 F7A 76.0(9) . . ?
F7B C20 C19 118.0(8) . . ?
F8A C20 C19 116.0(7) . . ?
F9 C20 C19 111.4(6) . . ?
F8B C20 C19 111.8(7) . . ?
F7A C20 C19 112.2(8) . . ?

_refine_diff_density_max         0.374
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_L-TBASO4_H2O
_database_code_depnum_ccdc_archive 'CCDC 1551280'
_audit_update_record             
;
2017-05-20 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'3(C24 H14 F12 N4 O2), 4(C16 H36 N), 2(O4 S), 2(O)'
_chemical_formula_sum            'C136 H186 F36 N16 O16 S2'
_chemical_formula_weight         3049.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.4903(8)
_cell_length_b                   22.6667(7)
_cell_length_c                   31.1019(13)
_cell_angle_alpha                90
_cell_angle_beta                 96.970(3)
_cell_angle_gamma                90
_cell_volume                     15738.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8266
_cell_measurement_theta_min      3.3970
_cell_measurement_theta_max      21.3660

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_F_000             6392.0
_exptl_transmission_factor_min   0.963
_exptl_transmission_factor_max   0.973
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.138
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71348
_diffrn_reflns_av_unetI/netI     0.1670
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.897
_diffrn_reflns_theta_max         28.876
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             38839
_reflns_number_gt                29512
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHEXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHEXTL'
_computing_publication_material  'Bruker SHEXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+0.0010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00013(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         38839
_refine_ls_number_parameters     1890
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.2880
_refine_ls_R_factor_gt           0.1072
_refine_ls_wR_factor_ref         0.3371
_refine_ls_wR_factor_gt          0.2547
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.002

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
S1 S 0.93241(6) 0.48465(6) 0.21138(6) 0.0737(4) Uani 1 1 d . . . . .
S2 S 0.43010(6) 0.33777(6) 0.27793(5) 0.0730(4) Uani 1 1 d . . . . .
O9 O 0.96329(14) 0.54277(14) 0.21404(13) 0.0838(11) Uani 1 1 d . . . . .
O8 O 0.97736(14) 0.43829(15) 0.22284(15) 0.0977(13) Uani 1 1 d . . . . .
O6 O 0.39241(16) 0.12214(15) 0.35916(12) 0.0787(11) Uani 1 1 d . . . . .
O13 O 0.38211(18) 0.32791(17) 0.30476(14) 0.1089(15) Uani 1 1 d . . . . .
O3 O 0.28081(15) 0.50770(17) 0.32962(13) 0.0868(12) Uani 1 1 d . . . . .
O7 O 0.90415(15) 0.47543(16) 0.16739(12) 0.0829(11) Uani 1 1 d . . . . .
O5 O 0.47176(19) -0.03467(18) 0.35130(13) 0.1025(14) Uani 1 1 d . . . . .
O11 O 0.46578(18) 0.28515(16) 0.27899(15) 0.1070(15) Uani 1 1 d . . . . .
O2 O 0.0965(2) 0.76243(17) 0.35870(14) 0.1061(15) Uani 1 1 d . . . . .
N11 N 0.42943(17) 0.17155(17) 0.30443(14) 0.0686(12) Uani 1 1 d . . . . .
H11N H 0.4366 0.2065 0.2957 0.082 Uiso 1 1 calc R U . . .
O10 O 0.88831(15) 0.48499(17) 0.24213(13) 0.0873(12) Uani 1 1 d . . . . .
N10 N 0.50172(19) -0.03148(19) 0.28447(16) 0.0782(13) Uani 1 1 d . . . . .
H10N H 0.5175 -0.0530 0.2661 0.094 Uiso 1 1 calc R U . . .
N12 N 0.38203(17) 0.22201(17) 0.35357(13) 0.0645(11) Uani 1 1 d . . . . .
H12N H 0.3900 0.2518 0.3382 0.077 Uiso 1 1 calc R U . . .
F26 F 0.6118(4) -0.3124(3) 0.3602(2) 0.268(5) Uani 1 1 d . . . . .
O1 O -0.0546(2) 0.63987(19) 0.35091(14) 0.1069(15) Uani 1 1 d . . . . .
O4 O 0.16692(16) 0.51941(19) 0.18816(15) 0.1049(15) Uani 1 1 d . . . . .
F11 F 0.1722(4) 1.0240(2) 0.4669(2) 0.243(4) Uani 1 1 d . . . . .
F21 F 0.1757(2) 0.7154(3) 0.0584(2) 0.192(3) Uani 1 1 d . . . . .
N6 N 0.29293(16) 0.4166(2) 0.30081(14) 0.0717(12) Uani 1 1 d . . . . .
H6N H 0.3188 0.3900 0.2963 0.086 Uiso 1 1 calc R U . . .
N3 N 0.04279(19) 0.82181(19) 0.30995(16) 0.0819(14) Uani 1 1 d . . . . .
H3N H 0.0318 0.8577 0.3047 0.098 Uiso 1 1 calc R U . . .
F18 F 0.3499(2) 0.6768(2) 0.3784(2) 0.180(2) Uani 1 1 d . . . . .
O14 O 0.4036(2) 0.3502(3) 0.23438(15) 0.143(2) Uani 1 1 d . . . . .
F30 F 0.5310(2) -0.1762(3) 0.51459(15) 0.184(2) Uani 1 1 d . . . . .
C64 C 0.4004(2) 0.1677(2) 0.34064(17) 0.0569(12) Uani 1 1 d . . . . .
N5 N 0.37404(17) 0.4669(2) 0.33236(14) 0.0764(13) Uani 1 1 d . . . . .
H5N H 0.3937 0.4382 0.3228 0.092 Uiso 1 1 calc R U . . .
N9 N 0.52855(19) -0.10894(19) 0.32804(14) 0.0782(13) Uani 1 1 d . . . . .
H9N H 0.5442 -0.1215 0.3059 0.094 Uiso 1 1 calc R U . . .
F10 F 0.2394(3) 0.9931(2) 0.5090(2) 0.213(3) Uani 1 1 d . . . . .
N1 N -0.0806(2) 0.55201(19) 0.31776(16) 0.0819(13) Uani 1 1 d . . . . .
H1N H -0.0886 0.5360 0.2926 0.098 Uiso 1 1 calc R U . . .
N7 N 0.09848(17) 0.4756(2) 0.22589(15) 0.0750(13) Uani 1 1 d . . . . .
H7N H 0.0613 0.4751 0.2298 0.090 Uiso 1 1 calc R U . . .
F9 F 0.3016(4) 0.7869(3) 0.5004(2) 0.256(4) Uani 1 1 d . . . . .
N8 N 0.06915(18) 0.5495(2) 0.17970(15) 0.0806(14) Uani 1 1 d . . . . .
H8N H 0.0355 0.5454 0.1899 0.097 Uiso 1 1 calc R U . . .
N16 N 0.72417(18) 0.4939(2) 0.18353(17) 0.0820(14) Uani 1 1 d . . . . .
F27 F 0.6751(2) -0.2765(2) 0.4033(2) 0.180(2) Uani 1 1 d . . . . .
F28 F 0.5016(3) -0.0967(2) 0.48780(16) 0.174(2) Uani 1 1 d . . . . .
F25 F 0.6117(3) -0.3243(2) 0.4249(2) 0.208(3) Uani 1 1 d . . . . .
C63 C 0.4631(2) 0.0685(2) 0.29649(16) 0.0585(13) Uani 1 1 d . . . . .
H63 H 0.4592 0.0600 0.3253 0.070 Uiso 1 1 calc R U . . .
C62 C 0.4489(2) 0.1240(2) 0.27975(17) 0.0602(13) Uani 1 1 d . . . . .
C10 C -0.0276(2) 0.6831(2) 0.2671(2) 0.0643(14) Uani 1 1 d . . . . .
F33B F 0.2959(4) 0.1850(3) 0.52631(18) 0.100(3) Uani 0.5 1 d . . P . .
N4 N 0.1048(2) 0.8624(2) 0.36471(16) 0.0852(14) Uani 1 1 d . . . . .
H4N H 0.0929 0.8951 0.3526 0.102 Uiso 1 1 calc R U . . .
C65 C 0.3516(2) 0.2336(2) 0.38930(17) 0.0636(14) Uani 1 1 d . . . . .
O12 O 0.4646(3) 0.3897(2) 0.2910(2) 0.167(2) Uani 1 1 d . . . . .
C57 C 0.4979(2) -0.0562(2) 0.3233(2) 0.0706(15) Uani 1 1 d . . . . .
C33 C 0.3125(2) 0.4668(3) 0.32089(19) 0.0689(15) Uani 1 1 d . . . . .
F29 F 0.4473(2) -0.1686(3) 0.47980(16) 0.194(3) Uani 1 1 d . . . . .
C39 C 0.1964(2) 0.4470(2) 0.26354(17) 0.0687(15) Uani 1 1 d . . . . .
H39 H 0.2127 0.4833 0.2575 0.082 Uiso 1 1 calc R U . . .
C14 C 0.0181(2) 0.7774(2) 0.2807(2) 0.0675(14) Uani 1 1 d . . . . .
F19 F 0.2208(2) 0.6395(2) 0.08603(18) 0.165(2) Uani 1 1 d . . . . .
F15A F 0.5848(5) 0.5482(5) 0.4506(6) 0.139(5) Uani 0.5 1 d . . P . .
C58 C 0.4830(2) 0.0258(2) 0.26988(18) 0.0653(14) Uani 1 1 d . . . . .
C31 C 0.4072(2) 0.5085(2) 0.35749(18) 0.0633(14) Uani 1 1 d . . . . .
C34 C 0.2318(2) 0.4056(2) 0.28678(18) 0.0677(14) Uani 1 1 d . . . . .
C17 C 0.1461(2) 0.8654(3) 0.4030(2) 0.0734(15) Uani 1 1 d . . . . .
C15 C -0.0048(2) 0.7252(2) 0.29607(19) 0.0683(14) Uani 1 1 d . . . . .
H15 H -0.0045 0.7191 0.3257 0.082 Uiso 1 1 calc R U . . .
C66 C 0.3396(2) 0.1921(3) 0.41959(16) 0.0701(15) Uani 1 1 d . . . . .
H66 H 0.3518 0.1532 0.4169 0.084 Uiso 1 1 calc R U . . .
C16 C 0.0827(2) 0.8114(3) 0.3458(2) 0.0753(16) Uani 1 1 d . . . . .
C72 C 0.3338(2) 0.2920(2) 0.39503(18) 0.0734(15) Uani 1 1 d . . . . .
H72 H 0.3411 0.3204 0.3748 0.088 Uiso 1 1 calc R U . . .
F34 F 0.2743(6) 0.3845(2) 0.4699(3) 0.292(5) Uani 1 1 d . . . . .
C56 C 0.5708(2) -0.1967(2) 0.3633(2) 0.0748(16) Uani 1 1 d . . . . .
H56 H 0.5861 -0.2069 0.3379 0.090 Uiso 1 1 calc R U . . .
C38 C 0.1367(2) 0.4352(3) 0.24896(18) 0.0703(15) Uani 1 1 d . . . . .
C55 C 0.5367(2) -0.1438(3) 0.3651(2) 0.0747(16) Uani 1 1 d . . . . .
C11 C -0.0287(2) 0.6926(2) 0.2224(2) 0.0754(15) Uani 1 1 d . . . . .
H11 H -0.0443 0.6643 0.2025 0.090 Uiso 1 1 calc R U . . .
C61 C 0.4536(2) 0.1375(3) 0.23680(19) 0.0811(17) Uani 1 1 d . . . . .
H61 H 0.4441 0.1750 0.2258 0.097 Uiso 1 1 calc R U . . .
F14 F 0.5692(2) 0.4576(3) 0.4239(3) 0.199(3) Uani 1 1 d . . . . .
C50 C 0.5810(2) -0.2321(2) 0.3983(2) 0.0732(16) Uani 1 1 d . . . . .
N13 N 0.5995(2) 0.2295(3) 0.3715(2) 0.1056(18) Uani 1 1 d . . . . .
C37 C 0.1132(2) 0.3797(3) 0.25790(19) 0.0818(17) Uani 1 1 d . . . . .
H37 H 0.0734 0.3710 0.2483 0.098 Uiso 1 1 calc R U . . .
C40 C 0.1162(3) 0.5157(3) 0.19771(19) 0.0751(16) Uani 1 1 d . . . . .
C41 C 0.0713(2) 0.5900(3) 0.14623(19) 0.0748(15) Uani 1 1 d . . . . .
C126 C 0.7616(2) 0.5962(3) 0.1626(2) 0.105(2) Uani 1 1 d . . . . .
H36D H 0.7430 0.6139 0.1859 0.126 Uiso 1 1 calc R U . . .
H36C H 0.7337 0.5988 0.1363 0.126 Uiso 1 1 calc R U . . .
N14 N 0.8612(3) 0.4252(3) 0.6203(2) 0.114(2) Uani 1 1 d D . . . .
C42 C 0.1248(2) 0.6140(3) 0.1349(2) 0.0813(17) Uani 1 1 d . . . . .
H41 H 0.1614 0.6026 0.1498 0.098 Uiso 1 1 calc R U . . .
C24 C 0.1485(2) 0.9180(3) 0.4261(2) 0.0804(16) Uani 1 1 d . . . . .
H24 H 0.1232 0.9492 0.4166 0.096 Uiso 1 1 calc R U . . .
C59 C 0.4860(3) 0.0378(3) 0.2269(2) 0.0840(17) Uani 1 1 d . . . . .
H59 H 0.4969 0.0084 0.2085 0.101 Uiso 1 1 calc R U . . .
F20 F 0.2084(2) 0.7111(3) 0.1247(2) 0.182(2) Uani 1 1 d . . . . .
C67 C 0.3093(2) 0.2086(3) 0.45404(19) 0.0788(16) Uani 1 1 d . . . . .
C30 C 0.3885(2) 0.5653(3) 0.3634(2) 0.0827(17) Uani 1 1 d . . . . .
H30 H 0.3513 0.5777 0.3501 0.099 Uiso 1 1 calc R U . . .
C18 C 0.1852(3) 0.8196(3) 0.4165(2) 0.0841(17) Uani 1 1 d . . . . .
H18 H 0.1842 0.7845 0.4010 0.101 Uiso 1 1 calc R U . . .
C48 C 0.0180(2) 0.6085(3) 0.12353(18) 0.0790(16) Uani 1 1 d . . . . .
H48 H -0.0180 0.5935 0.1307 0.095 Uiso 1 1 calc R U . . .
C32 C 0.4635(2) 0.4912(2) 0.37682(18) 0.0735(15) Uani 1 1 d . . . . .
H32 H 0.4769 0.4531 0.3727 0.088 Uiso 1 1 calc R U . . .
N15 N 0.8142(3) 0.8354(3) 0.3694(2) 0.117(2) Uani 1 1 d . . . . .
C12 C -0.0064(2) 0.7447(3) 0.2088(2) 0.0826(17) Uani 1 1 d . . . . .
H12 H -0.0072 0.7513 0.1792 0.099 Uiso 1 1 calc R U . . .
F4 F -0.0672(4) 0.5701(3) 0.48053(19) 0.216(3) Uani 1 1 d . . . . .
F13 F 0.6010(3) 0.5307(5) 0.4028(4) 0.298(6) Uani 1 1 d . . . . .
C13 C 0.0174(2) 0.7878(3) 0.2373(2) 0.0836(17) Uani 1 1 d . . . . .
H13 H 0.0324 0.8228 0.2272 0.100 Uiso 1 1 calc R U . . .
C26 C 0.4989(3) 0.5297(3) 0.4016(2) 0.0827(17) Uani 1 1 d . . . . .
C36 C 0.1488(2) 0.3383(3) 0.2809(2) 0.0882(19) Uani 1 1 d . . . . .
H36 H 0.1328 0.3017 0.2866 0.106 Uiso 1 1 calc R U . . .
C54 C 0.5154(2) -0.1307(3) 0.4038(2) 0.0823(17) Uani 1 1 d . . . . .
H54 H 0.4929 -0.0967 0.4060 0.099 Uiso 1 1 calc R U . . .
C125 C 0.7756(2) 0.5324(3) 0.1729(2) 0.093(2) Uani 1 1 d . . . . .
H35D H 0.8068 0.5311 0.1974 0.112 Uiso 1 1 calc R U . . .
H35C H 0.7920 0.5151 0.1484 0.112 Uiso 1 1 calc R U . . .
C28 C 0.4244(3) 0.6040(3) 0.3886(2) 0.0926(19) Uani 1 1 d . . . . .
C70 C 0.3058(3) 0.3079(3) 0.4302(2) 0.0853(18) Uani 1 1 d . . . . .
C35 C 0.2077(3) 0.3503(3) 0.2955(2) 0.0836(17) Uani 1 1 d . . . . .
H35 H 0.2314 0.3221 0.3111 0.100 Uiso 1 1 calc R U . . .
C51 C 0.5602(2) -0.2187(3) 0.4368(2) 0.0826(17) Uani 1 1 d . . . . .
H51 H 0.5682 -0.2432 0.4607 0.099 Uiso 1 1 calc R U . . .
C60 C 0.4727(3) 0.0939(3) 0.2112(2) 0.0953(19) Uani 1 1 d . . . . .
H60 H 0.4769 0.1023 0.1825 0.114 Uiso 1 1 calc R U . . .
C21 C 0.2270(3) 0.8787(3) 0.4765(2) 0.0904(19) Uani 1 1 d . . . . .
H21 H 0.2542 0.8833 0.5013 0.109 Uiso 1 1 calc R U . . .
F36 F 0.3183(5) 0.4063(2) 0.4191(4) 0.280(6) Uani 1 1 d . . . . .
C121 C 0.6744(2) 0.4919(3) 0.1463(2) 0.0931(19) Uani 1 1 d . . . . .
H31C H 0.6576 0.5312 0.1421 0.112 Uiso 1 1 calc R U . . .
H31D H 0.6430 0.4662 0.1542 0.112 Uiso 1 1 calc R U . . .
C52 C 0.5269(3) -0.1671(3) 0.4389(2) 0.0796(16) Uani 1 1 d . . . . .
C133 C 0.7517(3) 0.4336(3) 0.1940(3) 0.117(2) Uani 1 1 d . . . . .
H43D H 0.7826 0.4380 0.2184 0.140 Uiso 1 1 calc R U . . .
H43C H 0.7712 0.4208 0.1694 0.140 Uiso 1 1 calc R U . . .
C19 C 0.2255(3) 0.8273(3) 0.4534(2) 0.0822(17) Uani 1 1 d . . . . .
C129 C 0.6956(2) 0.5182(3) 0.2221(2) 0.094(2) Uani 1 1 d . . . . .
H39C H 0.6782 0.5564 0.2140 0.113 Uiso 1 1 calc R U . . .
H39D H 0.6629 0.4922 0.2274 0.113 Uiso 1 1 calc R U . . .
C43 C 0.1228(3) 0.6546(3) 0.1016(2) 0.0852(17) Uani 1 1 d . . . . .
C22 C 0.1882(3) 0.9236(3) 0.4627(2) 0.0854(18) Uani 1 1 d . . . . .
C46 C 0.0174(3) 0.6489(3) 0.0904(2) 0.094(2) Uani 1 1 d . . . . .
C105 C 0.8217(3) 0.7916(3) 0.4073(2) 0.118(2) Uani 1 1 d . . . . .
H15C H 0.7845 0.7696 0.4063 0.142 Uiso 1 1 calc R U . . .
H15D H 0.8255 0.8145 0.4338 0.142 Uiso 1 1 calc R U . . .
C27 C 0.4809(3) 0.5873(3) 0.40867(19) 0.0874(18) Uani 1 1 d . . . . .
H27 H 0.5052 0.6134 0.4259 0.105 Uiso 1 1 calc R U . . .
C69 C 0.2922(3) 0.2662(3) 0.4592(2) 0.0900(19) Uani 1 1 d . . . . .
H69 H 0.2715 0.2767 0.4822 0.108 Uiso 1 1 calc R U . . .
C7 C -0.0891(3) 0.5175(3) 0.3527(2) 0.0902(19) Uani 1 1 d . . . . .
F5 F -0.0747(6) 0.4827(3) 0.5020(2) 0.303(6) Uani 1 1 d . . . . .
C49 C 0.6183(4) -0.2856(3) 0.3942(3) 0.109(2) Uani 1 1 d . . . . .
F8 F 0.3011(5) 0.7685(5) 0.4423(3) 0.300(6) Uani 1 1 d . . . . .
F23 F -0.0428(3) 0.6702(5) 0.0253(2) 0.251(4) Uani 1 1 d . . . . .
F31 F 0.3327(4) 0.1257(4) 0.4960(3) 0.247(4) Uani 1 1 d . . . . .
F17 F 0.4080(5) 0.6835(5) 0.4321(3) 0.335(8) Uani 1 1 d . . . . .
C117 C 0.8716(4) 0.8717(3) 0.3672(2) 0.125(3) Uani 1 1 d . . . . .
H27D H 0.9034 0.8453 0.3611 0.150 Uiso 1 1 calc R U . . .
H27C H 0.8647 0.8993 0.3433 0.150 Uiso 1 1 calc R U . . .
C4 C -0.0955(4) 0.4982(4) 0.4280(3) 0.128(3) Uani 1 1 d . . . . .
C78 C 0.5452(3) 0.2893(4) 0.4260(2) 0.115(2) Uani 1 1 d . . . . .
H78B H 0.5589 0.2623 0.4494 0.138 Uiso 1 1 calc R U . . .
H78A H 0.5740 0.3212 0.4264 0.138 Uiso 1 1 calc R U . . .
C68 C 0.2941(5) 0.1648(4) 0.4864(4) 0.119(3) Uani 1 1 d . . . . .
C6 C -0.0870(3) 0.5385(3) 0.3949(2) 0.109(2) Uani 1 1 d . . . . .
H6 H -0.0801 0.5782 0.4010 0.130 Uiso 1 1 calc R U . . .
C2 C -0.1077(4) 0.4191(4) 0.3775(4) 0.143(3) Uani 1 1 d . . . . .
C98 C 0.8979(4) 0.3461(4) 0.5702(3) 0.146(3) Uani 1 1 d D . . . .
H98B H 0.8649 0.3505 0.5473 0.176 Uiso 1 1 calc R U . . .
H98A H 0.8866 0.3160 0.5899 0.176 Uiso 1 1 calc R U . . .
C79 C 0.4853(3) 0.3137(4) 0.4330(3) 0.134(3) Uani 1 1 d . . . . .
H79B H 0.4716 0.3397 0.4091 0.161 Uiso 1 1 calc R U . . .
H79A H 0.4570 0.2814 0.4326 0.161 Uiso 1 1 calc R U . . .
C122 C 0.6934(3) 0.4703(4) 0.1030(2) 0.125(3) Uani 1 1 d . . . . .
H32D H 0.7180 0.5002 0.0915 0.150 Uiso 1 1 calc R U . . .
H32C H 0.7173 0.4348 0.1080 0.150 Uiso 1 1 calc R U . . .
C73 C 0.6216(3) 0.1812(4) 0.4041(3) 0.129(3) Uani 1 1 d . . . . .
H73A H 0.6618 0.1699 0.3991 0.155 Uiso 1 1 calc R U . . .
H73B H 0.6243 0.1978 0.4330 0.155 Uiso 1 1 calc R U . . .
C127 C 0.8185(3) 0.6292(3) 0.1565(3) 0.134(3) Uani 1 1 d . . . . .
H37D H 0.8470 0.6235 0.1822 0.161 Uiso 1 1 calc R U . . .
H37C H 0.8356 0.6118 0.1323 0.161 Uiso 1 1 calc R U . . .
C45 C 0.0691(3) 0.6727(3) 0.0794(2) 0.105(2) Uani 1 1 d . . . . .
H45 H 0.0681 0.7006 0.0573 0.127 Uiso 1 1 calc R U . . .
C8 C -0.0994(3) 0.4561(3) 0.3448(3) 0.120(3) Uani 1 1 d . . . . .
H8 H -0.1005 0.4415 0.3168 0.144 Uiso 1 1 calc R U . . .
C53 C 0.5033(4) -0.1523(5) 0.4805(3) 0.119(3) Uani 1 1 d . . . . .
C113 C 0.7600(4) 0.8741(4) 0.3753(3) 0.132(3) Uani 1 1 d . . . . .
H23D H 0.7270 0.8484 0.3801 0.159 Uiso 1 1 calc R U . . .
H23C H 0.7698 0.8974 0.4014 0.159 Uiso 1 1 calc R U . . .
C128 C 0.8110(3) 0.6934(4) 0.1487(3) 0.145(3) Uani 1 1 d . . . . .
H38C H 0.7982 0.7002 0.1185 0.218 Uiso 1 1 calc R U . . .
H38E H 0.8486 0.7130 0.1568 0.218 Uiso 1 1 calc R U . . .
H38D H 0.7816 0.7086 0.1656 0.218 Uiso 1 1 calc R U . . .
C77 C 0.5417(3) 0.2568(3) 0.3828(2) 0.114(2) Uani 1 1 d . . . . .
H77A H 0.5273 0.2843 0.3600 0.137 Uiso 1 1 calc R U . . .
H77B H 0.5121 0.2257 0.3829 0.137 Uiso 1 1 calc R U . . .
C130 C 0.7353(3) 0.5254(3) 0.2633(2) 0.111(2) Uani 1 1 d . . . . .
H40C H 0.7684 0.5513 0.2588 0.133 Uiso 1 1 calc R U . . .
H40D H 0.7518 0.4873 0.2728 0.133 Uiso 1 1 calc R U . . .
C97 C 0.9063(3) 0.4040(4) 0.5947(3) 0.151(3) Uani 1 1 d D . . . .
H97B H 0.9120 0.4344 0.5736 0.181 Uiso 1 1 calc R U . . .
H97A H 0.9436 0.4011 0.6139 0.181 Uiso 1 1 calc R U . . .
F15B F 0.5553(8) 0.5087(10) 0.4687(5) 0.218(8) Uani 0.5 1 d . . P . .
C80 C 0.4848(4) 0.3476(4) 0.4750(3) 0.151(3) Uani 1 1 d . . . . .
H80A H 0.4961 0.3217 0.4991 0.226 Uiso 1 1 calc R U . . .
H80C H 0.4453 0.3627 0.4768 0.226 Uiso 1 1 calc R U . . .
H80B H 0.5127 0.3797 0.4758 0.226 Uiso 1 1 calc R U . . .
C114 C 0.7388(5) 0.9155(4) 0.3388(4) 0.164(4) Uani 1 1 d . . . . .
H24C H 0.7716 0.9405 0.3324 0.197 Uiso 1 1 calc R U . . .
H24D H 0.7247 0.8931 0.3130 0.197 Uiso 1 1 calc R U . . .
C85 C 0.5863(3) 0.2065(4) 0.3261(2) 0.127(3) Uani 1 1 d . . . . .
H85A H 0.5713 0.2388 0.3074 0.152 Uiso 1 1 calc R U . . .
H85B H 0.5547 0.1773 0.3254 0.152 Uiso 1 1 calc R U . . .
F7 F 0.2451(4) 0.7298(3) 0.4663(5) 0.350(9) Uani 1 1 d . . . . .
C109 C 0.8054(4) 0.8031(4) 0.3256(3) 0.140(3) Uani 1 1 d . . . . .
H19D H 0.8018 0.8330 0.3031 0.168 Uiso 1 1 calc R U . . .
H19C H 0.8418 0.7813 0.3230 0.168 Uiso 1 1 calc R U . . .
C74 C 0.5836(3) 0.1263(4) 0.4029(3) 0.139(3) Uani 1 1 d D . . . .
H74A H 0.5772 0.1105 0.3737 0.166 Uiso 1 1 calc R U . . .
H74B H 0.5450 0.1351 0.4123 0.166 Uiso 1 1 calc R U . . .
C123 C 0.6396(3) 0.4576(4) 0.0701(3) 0.141(3) Uani 1 1 d . . . . .
H33C H 0.6536 0.4426 0.0439 0.169 Uiso 1 1 calc R U . . .
H33D H 0.6159 0.4268 0.0814 0.169 Uiso 1 1 calc R U . . .
C99 C 0.9500(4) 0.3256(4) 0.5513(3) 0.157(4) Uani 1 1 d . . . . .
H99A H 0.9820 0.3187 0.5745 0.188 Uiso 1 1 calc R U . . .
H99B H 0.9629 0.3570 0.5333 0.188 Uiso 1 1 calc R U . . .
C3 C -0.1058(5) 0.4399(4) 0.4201(4) 0.163(4) Uani 1 1 d . . . . .
H3 H -0.1115 0.4143 0.4426 0.196 Uiso 1 1 calc R U . . .
C86 C 0.6389(4) 0.1792(5) 0.3079(3) 0.167(4) Uani 1 1 d . . . . .
H86A H 0.6688 0.2092 0.3049 0.200 Uiso 1 1 calc R U . . .
H86B H 0.6569 0.1494 0.3278 0.200 Uiso 1 1 calc R U . . .
C131 C 0.7015(3) 0.5507(4) 0.2977(3) 0.140(3) Uani 1 1 d . . . . .
H41D H 0.6679 0.5251 0.3011 0.169 Uiso 1 1 calc R U . . .
H41C H 0.6855 0.5888 0.2878 0.169 Uiso 1 1 calc R U . . .
C20 C 0.2639(4) 0.7737(5) 0.4747(5) 0.202(6) Uani 1 1 d . . . . .
C119 C 0.9565(5) 0.9302(5) 0.4054(3) 0.178(4) Uani 1 1 d . . . . .
H29C H 0.9833 0.8973 0.4026 0.214 Uiso 1 1 calc R U . . .
H29D H 0.9557 0.9542 0.3795 0.214 Uiso 1 1 calc R U . . .
C118 C 0.8924(4) 0.9061(4) 0.4086(3) 0.147(3) Uani 1 1 d . . . . .
H28D H 0.8652 0.9385 0.4119 0.177 Uiso 1 1 calc R U . . .
H28C H 0.8929 0.8804 0.4336 0.177 Uiso 1 1 calc R U . . .
F6 F -0.1490(5) 0.5330(5) 0.4819(3) 0.314(6) Uani 1 1 d . . . . .
C23 C 0.1891(4) 0.9782(4) 0.4874(4) 0.136(3) Uani 1 1 d . . . . .
C110 C 0.7524(4) 0.7599(4) 0.3152(3) 0.174(4) Uani 1 1 d D . . . .
H20D H 0.7503 0.7331 0.3393 0.209 Uiso 1 1 calc R U . . .
H20C H 0.7150 0.7816 0.3103 0.209 Uiso 1 1 calc R U . . .
C44 C 0.1800(4) 0.6796(5) 0.0902(4) 0.127(3) Uani 1 1 d . . . . .
C76 C 0.5832(5) 0.0232(4) 0.4331(4) 0.201(5) Uani 1 1 d D . . . .
H76A H 0.5446 0.0301 0.4423 0.301 Uiso 1 1 calc R U . . .
H76C H 0.6050 -0.0046 0.4523 0.301 Uiso 1 1 calc R U . . .
H76B H 0.5782 0.0075 0.4042 0.301 Uiso 1 1 calc R U . . .
C124 C 0.6012(4) 0.5085(4) 0.0589(3) 0.140(3) Uani 1 1 d . . . . .
H34C H 0.5913 0.5269 0.0849 0.210 Uiso 1 1 calc R U . . .
H34D H 0.5651 0.4959 0.0417 0.210 Uiso 1 1 calc R U . . .
H34E H 0.6219 0.5363 0.0427 0.210 Uiso 1 1 calc R U . . .
C111 C 0.7622(6) 0.7271(6) 0.2766(3) 0.314(11) Uani 1 1 d D . . . .
H21D H 0.7774 0.7524 0.2553 0.377 Uiso 1 1 calc R U . . .
H21C H 0.7896 0.6945 0.2834 0.377 Uiso 1 1 calc R U . . .
F12 F 0.1532(4) 0.9773(3) 0.5158(3) 0.264(5) Uani 1 1 d . . . . .
C75 C 0.6181(4) 0.0816(4) 0.4339(3) 0.155(3) Uani 1 1 d D . . . .
H75B H 0.6574 0.0747 0.4250 0.187 Uiso 1 1 calc R U . . .
H75A H 0.6234 0.0975 0.4631 0.187 Uiso 1 1 calc R U . . .
F33A F 0.2669(7) 0.1182(6) 0.4656(3) 0.139(4) Uani 0.5 1 d . . P . .
C132 C 0.7383(4) 0.5587(5) 0.3416(3) 0.180(4) Uani 1 1 d . . . . .
H42E H 0.7578 0.5222 0.3504 0.271 Uiso 1 1 calc R U . . .
H42D H 0.7124 0.5701 0.3625 0.271 Uiso 1 1 calc R U . . .
H42C H 0.7679 0.5888 0.3396 0.271 Uiso 1 1 calc R U . . .
F16 F 0.4361(4) 0.7025(3) 0.3762(5) 0.299(7) Uani 1 1 d . . . . .
C101 C 0.8705(5) 0.4899(5) 0.6304(4) 0.175(4) Uani 1 1 d . . . . .
H11D H 0.8542 0.5109 0.6044 0.210 Uiso 1 1 calc R U . . .
H11C H 0.8446 0.4991 0.6522 0.210 Uiso 1 1 calc R U . . .
C115 C 0.6893(5) 0.9524(5) 0.3520(4) 0.182(4) Uani 1 1 d . . . . .
H25C H 0.7033 0.9735 0.3784 0.219 Uiso 1 1 calc R U . . .
H25D H 0.6564 0.9271 0.3579 0.219 Uiso 1 1 calc R U . . .
C5 C -0.0926(8) 0.5198(6) 0.4731(5) 0.185(5) Uani 1 1 d . . . . .
F35 F 0.2422(5) 0.3831(4) 0.4131(5) 0.311(6) Uani 1 1 d . . . . .
C120 C 0.9796(5) 0.9655(6) 0.4430(4) 0.221(5) Uani 1 1 d . . . . .
H30D H 0.9513 0.9958 0.4476 0.332 Uiso 1 1 calc R U . . .
H30E H 1.0169 0.9832 0.4381 0.332 Uiso 1 1 calc R U . . .
H30C H 0.9858 0.9406 0.4681 0.332 Uiso 1 1 calc R U . . .
C93 C 0.7949(3) 0.4142(5) 0.6019(4) 0.199(5) Uani 1 1 d D . . . .
H93A H 0.7882 0.3721 0.5985 0.239 Uiso 1 1 calc R U . . .
H93B H 0.7691 0.4287 0.6224 0.239 Uiso 1 1 calc R U . . .
F24 F -0.0849(3) 0.6366(4) 0.0708(3) 0.270(5) Uani 1 1 d . . . . .
C94 C 0.7805(5) 0.4410(6) 0.5635(3) 0.209(6) Uani 1 1 d D . . . .
H94A H 0.8059 0.4261 0.5428 0.251 Uiso 1 1 calc R U . . .
H94B H 0.7876 0.4831 0.5667 0.251 Uiso 1 1 calc R U . . .
F22 F -0.0559(4) 0.7181(4) 0.0757(4) 0.314(7) Uani 1 1 d . . . . .
C100 C 0.9423(5) 0.2744(6) 0.5262(4) 0.279(8) Uani 1 1 d . . . . .
H10E H 0.9385 0.2411 0.5447 0.419 Uiso 1 1 calc R U . . .
H10D H 0.9764 0.2690 0.5108 0.419 Uiso 1 1 calc R U . . .
H10C H 0.9068 0.2780 0.5059 0.419 Uiso 1 1 calc R U . . .
F32 F 0.2417(5) 0.1622(5) 0.4911(5) 0.311(6) Uani 1 1 d . . . . .
C9 C -0.0605(2) 0.6096(3) 0.3185(2) 0.0786(16) Uani 1 1 d . . . . .
N2 N -0.04959(18) 0.62704(19) 0.27820(16) 0.0778(13) Uani 1 1 d . . . . .
H2N H -0.0567 0.6017 0.2576 0.093 Uiso 1 1 calc R U . . .
C116 C 0.6673(5) 0.9958(6) 0.3171(5) 0.239(6) Uani 1 1 d . . . . .
H26C H 0.6919 1.0306 0.3201 0.358 Uiso 1 1 calc R U . . .
H26E H 0.6266 1.0063 0.3198 0.358 Uiso 1 1 calc R U . . .
H26D H 0.6694 0.9784 0.2893 0.358 Uiso 1 1 calc R U . . .
C95 C 0.7139(5) 0.4302(6) 0.5460(4) 0.261(8) Uani 1 1 d D . . . .
H95B H 0.7050 0.3884 0.5475 0.313 Uiso 1 1 calc R U . . .
H95A H 0.6884 0.4510 0.5640 0.313 Uiso 1 1 calc R U . . .
C87 C 0.6205(5) 0.1520(6) 0.2657(4) 0.213(6) Uani 1 1 d . . . . .
H87A H 0.6067 0.1822 0.2447 0.256 Uiso 1 1 calc R U . . .
H87B H 0.5877 0.1248 0.2678 0.256 Uiso 1 1 calc R U . . .
C108 C 0.8193(5) 0.6713(6) 0.4482(6) 0.353(11) Uani 1 1 d D . . . .
H18D H 0.7849 0.6936 0.4363 0.529 Uiso 1 1 calc R U . . .
H18C H 0.8134 0.6574 0.4766 0.529 Uiso 1 1 calc R U . . .
H18E H 0.8247 0.6383 0.4298 0.529 Uiso 1 1 calc R U . . .
C106 C 0.8725(4) 0.7468(4) 0.4115(3) 0.166(4) Uani 1 1 d D . . . .
H16D H 0.9104 0.7675 0.4122 0.199 Uiso 1 1 calc R U . . .
H16C H 0.8683 0.7213 0.3863 0.199 Uiso 1 1 calc R U . . .
C96 C 0.7007(7) 0.4518(9) 0.4986(5) 0.388(14) Uani 1 1 d D . . . .
H96C H 0.7365 0.4681 0.4894 0.582 Uiso 1 1 calc R U . . .
H96A H 0.6701 0.4814 0.4967 0.582 Uiso 1 1 calc R U . . .
H96B H 0.6874 0.4191 0.4802 0.582 Uiso 1 1 calc R U . . .
F2 F -0.1548(10) 0.3471(7) 0.3371(8) 0.390(12) Uani 1 1 d . . . . .
F1 F -0.1394(8) 0.3281(3) 0.3967(4) 0.352(7) Uani 1 1 d . . . . .
F3 F -0.0697(6) 0.3304(4) 0.3642(6) 0.348(7) Uani 1 1 d . . . . .
C29 C 0.4026(5) 0.6652(4) 0.3915(6) 0.175(5) Uani 1 1 d . . . . .
C25 C 0.5604(4) 0.5135(5) 0.4251(5) 0.139(4) Uani 1 1 d . . . . .
C88 C 0.6726(8) 0.1200(9) 0.2513(5) 0.372(11) Uani 1 1 d . . . . .
H88A H 0.6655 0.1133 0.2206 0.558 Uiso 1 1 calc R U . . .
H88C H 0.6775 0.0828 0.2661 0.558 Uiso 1 1 calc R U . . .
H88B H 0.7082 0.1432 0.2580 0.558 Uiso 1 1 calc R U . . .
C71 C 0.2984(7) 0.3741(5) 0.4407(5) 0.225(7) Uani 1 1 d . . . . .
C47 C -0.0404(4) 0.6664(6) 0.0648(4) 0.150(4) Uani 1 1 d . . . . .
C1 C -0.1185(9) 0.3516(10) 0.3620(11) 0.274(16) Uani 1 1 d . . . . .
C112 C 0.7022(5) 0.7066(6) 0.2619(4) 0.331(10) Uani 1 1 d D . . . .
H22C H 0.6904 0.6778 0.2819 0.497 Uiso 1 1 calc R U . . .
H22E H 0.7015 0.6890 0.2338 0.497 Uiso 1 1 calc R U . . .
H22D H 0.6749 0.7393 0.2603 0.497 Uiso 1 1 calc R U . . .
C107 C 0.8736(5) 0.7098(4) 0.4514(4) 0.242(7) Uani 1 1 d D . . . .
H17D H 0.9094 0.6856 0.4548 0.290 Uiso 1 1 calc R U . . .
H17C H 0.8746 0.7351 0.4767 0.290 Uiso 1 1 calc R U . . .
C135 C 0.7512(8) 0.3292(4) 0.2207(6) 0.318(12) Uani 1 1 d D . . . .
H45D H 0.7937 0.3356 0.2201 0.382 Uiso 1 1 calc R U . . .
H45C H 0.7431 0.3129 0.2482 0.382 Uiso 1 1 calc R U . . .
C134 C 0.7096(4) 0.3855(4) 0.2047(4) 0.175(4) Uani 1 1 d . . . . .
H44D H 0.6821 0.3753 0.1793 0.211 Uiso 1 1 calc R U . . .
H44C H 0.6865 0.3982 0.2274 0.211 Uiso 1 1 calc R U . . .
C136 C 0.7199(13) 0.2961(9) 0.1806(7) 0.61(3) Uani 1 1 d D . . . .
H46C H 0.7493 0.2747 0.1669 0.911 Uiso 1 1 calc R U . . .
H46E H 0.7000 0.3240 0.1605 0.911 Uiso 1 1 calc R U . . .
H46D H 0.6910 0.2689 0.1896 0.911 Uiso 1 1 calc R U . . .
C103 C 0.9353(7) 0.5805(5) 0.6431(5) 0.254(7) Uani 1 1 d D . . . .
H13D H 0.9070 0.6004 0.6593 0.304 Uiso 1 1 calc R U . . .
H13C H 0.9749 0.5864 0.6587 0.304 Uiso 1 1 calc R U . . .
C102 C 0.9215(7) 0.5144(9) 0.6432(6) 0.329(11) Uani 1 1 d . . . . .
H12D H 0.9501 0.4961 0.6265 0.394 Uiso 1 1 calc R U . . .
H12C H 0.9321 0.5015 0.6729 0.394 Uiso 1 1 calc R U . . .
C104 C 0.9334(8) 0.6105(8) 0.5993(4) 0.328(11) Uani 1 1 d D . . . .
H14D H 0.9192 0.5831 0.5769 0.491 Uiso 1 1 calc R U . . .
H14C H 0.9729 0.6235 0.5952 0.491 Uiso 1 1 calc R U . . .
H14E H 0.9070 0.6439 0.5983 0.491 Uiso 1 1 calc R U . . .
C91 C 0.8583(5) 0.3449(7) 0.7397(4) 0.248(10) Uani 1 1 d D . . . .
H91A H 0.8895 0.3165 0.7361 0.298 Uiso 1 1 calc R U . . .
H91B H 0.8738 0.3735 0.7614 0.298 Uiso 1 1 calc R U . . .
C90 C 0.8391(6) 0.3742(6) 0.6989(3) 0.281(11) Uani 1 1 d D . . . .
H90B H 0.8045 0.3511 0.6874 0.337 Uiso 1 1 calc R U . . .
H90A H 0.8227 0.4110 0.7082 0.337 Uiso 1 1 calc R U . . .
C89 C 0.8644(6) 0.3915(5) 0.6602(3) 0.266(8) Uani 1 1 d D . . . .
H89A H 0.8714 0.3526 0.6487 0.320 Uiso 1 1 calc R U . . .
H89B H 0.9037 0.4040 0.6733 0.320 Uiso 1 1 calc R U . . .
O16 O 0.5672(13) 0.2748(15) 0.2286(6) 0.69(3) Uani 1 1 d . . . . .
C81 C 0.6493(3) 0.2756(4) 0.3757(3) 0.143(3) Uani 1 1 d . . . . .
H81A H 0.6855 0.2581 0.3672 0.171 Uiso 1 1 calc R U . . .
H81B H 0.6577 0.2875 0.4058 0.171 Uiso 1 1 calc R U . . .
C82 C 0.6329(6) 0.3307(6) 0.3477(6) 0.245(7) Uani 1 1 d D . . . .
H82B H 0.6206 0.3177 0.3182 0.294 Uiso 1 1 calc R U . . .
H82A H 0.5986 0.3494 0.3580 0.294 Uiso 1 1 calc R U . . .
C84 C 0.7089(13) 0.3926(15) 0.3875(11) 0.47(2) Uani 1 1 d . . . . .
H84B H 0.7355 0.3615 0.3986 0.710 Uiso 1 1 calc R U . . .
H84A H 0.6784 0.3978 0.4063 0.710 Uiso 1 1 calc R U . . .
H84C H 0.7311 0.4286 0.3863 0.710 Uiso 1 1 calc R U . . .
C83 C 0.6825(12) 0.3780(12) 0.3464(9) 0.45(2) Uani 1 1 d D . . . .
H83A H 0.6652 0.4131 0.3321 0.545 Uiso 1 1 calc R U . . .
H83B H 0.7129 0.3631 0.3296 0.545 Uiso 1 1 calc R U . . .
O15 O 0.5887(10) 0.373(3) 0.2688(17) 1.22(6) Uani 1 1 d . . . . .
C92 C 0.8213(11) 0.3239(13) 0.7491(10) 0.55(3) Uani 1 1 d . . . . .
H92A H 0.8006 0.3502 0.7664 0.825 Uiso 1 1 calc R U . . .
H92B H 0.8338 0.2894 0.7658 0.825 Uiso 1 1 calc R U . . .
H92C H 0.7949 0.3124 0.7239 0.825 Uiso 1 1 calc R U . . .


_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
S1 O7 1.452(4) . ?
S1 O10 1.459(4) . ?
S1 O8 1.472(3) . ?
S1 O9 1.487(3) . ?
S2 O11 1.435(4) . ?
S2 O12 1.442(5) . ?
S2 O14 1.440(5) . ?
S2 O13 1.459(3) . ?
O6 C64 1.207(5) . ?
O3 C33 1.220(6) . ?
O5 C57 1.212(6) . ?
O2 C16 1.207(6) . ?
N11 C64 1.371(6) . ?
N11 C62 1.424(6) . ?
N10 C57 1.343(6) . ?
N10 C58 1.421(6) . ?
N12 C64 1.374(6) . ?
N12 C65 1.398(6) . ?
F26 C49 1.214(9) . ?
O1 C9 1.213(6) . ?
O4 C40 1.217(6) . ?
F11 C23 1.253(11) . ?
F21 C44 1.275(9) . ?
N6 C33 1.345(6) . ?
N6 C34 1.414(6) . ?
N3 C16 1.365(7) . ?
N3 C14 1.423(6) . ?
F18 C29 1.234(9) . ?
F30 C53 1.284(8) . ?
N5 C31 1.384(6) . ?
N5 C33 1.388(6) . ?
N9 C57 1.378(6) . ?
N9 C55 1.391(6) . ?
F10 C23 1.288(8) . ?
N1 C9 1.382(7) . ?
N1 C7 1.370(7) . ?
N7 C40 1.355(6) . ?
N7 C38 1.394(6) . ?
F9 C20 1.133(9) . ?
N8 C40 1.370(6) . ?
N8 C41 1.393(6) . ?
N16 C133 1.518(7) . ?
N16 C121 1.510(7) . ?
N16 C125 1.518(6) . ?
N16 C129 1.533(7) . ?
F27 C49 1.290(8) . ?
F28 C53 1.283(9) . ?
F25 C49 1.318(8) . ?
C63 C58 1.383(6) . ?
C63 C62 1.383(6) . ?
C62 C61 1.387(7) . ?
C10 C15 1.370(6) . ?
C10 C11 1.403(7) . ?
C10 N2 1.421(6) . ?
F33B C68 1.319(11) . ?
N4 C16 1.364(6) . ?
N4 C17 1.421(7) . ?
C65 C66 1.381(6) . ?
C65 C72 1.401(7) . ?
F29 C53 1.309(9) . ?
C39 C34 1.377(7) . ?
C39 C38 1.390(6) . ?
C14 C13 1.371(7) . ?
C14 C15 1.396(7) . ?
F19 C44 1.309(8) . ?
F15A C25 1.203(15) . ?
C58 C59 1.374(7) . ?
C31 C30 1.373(7) . ?
C31 C32 1.391(7) . ?
C34 C35 1.403(7) . ?
C17 C24 1.390(7) . ?
C17 C18 1.391(7) . ?
C66 C67 1.389(7) . ?
C72 C70 1.376(7) . ?
F34 C71 1.138(8) . ?
C56 C50 1.349(7) . ?
C56 C55 1.428(7) . ?
C38 C37 1.403(7) . ?
C55 C54 1.380(7) . ?
C11 C12 1.371(7) . ?
C61 C60 1.371(7) . ?
F14 C25 1.282(11) . ?
C50 C51 1.370(7) . ?
C50 C49 1.488(8) . ?
N13 C85 1.500(8) . ?
N13 C73 1.535(9) . ?
N13 C77 1.520(7) . ?
N13 C81 1.526(9) . ?
C37 C36 1.376(7) . ?
C41 C48 1.380(7) . ?
C41 C42 1.404(7) . ?
C126 C125 1.506(7) . ?
C126 C127 1.513(8) . ?
N14 C97 1.446(8) . ?
N14 C93 1.5492(10) . ?
N14 C101 1.509(11) . ?
N14 C89 1.4504(10) . ?
C42 C43 1.382(7) . ?
C24 C22 1.366(8) . ?
C59 C60 1.382(7) . ?
F20 C44 1.381(10) . ?
C67 C69 1.377(7) . ?
C67 C68 1.485(9) . ?
C30 C28 1.372(7) . ?
C18 C19 1.385(8) . ?
C48 C46 1.376(7) . ?
C32 C26 1.358(7) . ?
N15 C113 1.531(9) . ?
N15 C105 1.535(8) . ?
N15 C109 1.538(9) . ?
N15 C117 1.539(8) . ?
C12 C13 1.381(7) . ?
F4 C5 1.284(12) . ?
F13 C25 1.276(13) . ?
C26 C27 1.392(8) . ?
C26 C25 1.528(10) . ?
C36 C35 1.374(7) . ?
C54 C52 1.369(7) . ?
C28 C27 1.398(8) . ?
C28 C29 1.477(11) . ?
C70 C69 1.365(7) . ?
C70 C71 1.549(13) . ?
C51 C52 1.394(8) . ?
C21 C22 1.375(8) . ?
C21 C19 1.368(8) . ?
F36 C71 1.121(10) . ?
C121 C122 1.541(8) . ?
C52 C53 1.494(9) . ?
C133 C134 1.509(9) . ?
C19 C20 1.587(13) . ?
C129 C130 1.480(8) . ?
C43 C45 1.380(8) . ?
C43 C44 1.488(9) . ?
C22 C23 1.455(9) . ?
C46 C45 1.362(8) . ?
C46 C47 1.493(11) . ?
C105 C106 1.522(9) . ?
C7 C6 1.391(8) . ?
C7 C8 1.427(8) . ?
F5 C5 1.259(14) . ?
F8 C20 1.390(15) . ?
F23 C47 1.226(11) . ?
F31 C68 1.250(9) . ?
F17 C29 1.321(16) . ?
C117 C118 1.527(9) . ?
C4 C3 1.359(11) . ?
C4 C6 1.406(9) . ?
C4 C5 1.480(14) . ?
C78 C79 1.497(8) . ?
C78 C77 1.525(8) . ?
C68 F32 1.207(10) . ?
C68 F33A 1.347(12) . ?
C2 C8 1.349(10) . ?
C2 C3 1.403(12) . ?
C2 C1 1.61(3) . ?
C98 C97 1.5186(10) . ?
C98 C99 1.449(9) . ?
C79 C80 1.517(9) . ?
C122 C123 1.515(9) . ?
C73 C74 1.507(9) . ?
C127 C128 1.482(9) . ?
C113 C114 1.504(10) . ?
C130 C131 1.499(9) . ?
F15B C25 1.378(17) . ?
C114 C115 1.490(11) . ?
C85 C86 1.504(9) . ?
F7 C20 1.100(10) . ?
C109 C110 1.545(10) . ?
C74 C75 1.5399(10) . ?
C123 C124 1.458(9) . ?
C99 C100 1.396(11) . ?
C86 C87 1.463(12) . ?
C131 C132 1.519(10) . ?
C119 C120 1.461(12) . ?
C119 C118 1.555(11) . ?
F6 C5 1.363(16) . ?
C23 F12 1.268(11) . ?
C110 C111 1.4513(10) . ?
C76 C75 1.5392(10) . ?
C111 C112 1.4490(10) . ?
F16 C29 1.263(14) . ?
C101 C102 1.295(14) . ?
C115 C116 1.504(13) . ?
F35 C71 1.455(17) . ?
C93 C94 1.346(13) . ?
F24 C47 1.241(11) . ?
C94 C95 1.5499(10) . ?
F22 C47 1.280(13) . ?
C9 N2 1.364(7) . ?
C95 C96 1.5494(10) . ?
C87 C88 1.493(17) . ?
C108 C107 1.4945(7) . ?
C106 C107 1.4953(7) . ?
F2 C1 1.06(3) . ?
F1 C1 1.34(3) . ?
F3 C1 1.191(19) . ?
C135 C136 1.5499(11) . ?
C135 C134 1.623(14) . ?
C103 C104 1.5194(10) . ?
C103 C102 1.529(17) . ?
C91 C92 1.03(2) . ?
C91 C90 1.4500(10) . ?
C90 C89 1.4487(10) . ?
C81 C82 1.541(14) . ?
C82 C83 1.5502(12) . ?
C84 C83 1.38(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
O7 S1 O10 111.3(2) . . ?
O7 S1 O8 109.5(2) . . ?
O10 S1 O8 110.3(2) . . ?
O7 S1 O9 109.2(3) . . ?
O10 S1 O9 108.0(2) . . ?
O8 S1 O9 108.5(2) . . ?
O11 S2 O12 113.1(3) . . ?
O11 S2 O14 110.5(3) . . ?
O12 S2 O14 104.6(4) . . ?
O11 S2 O13 108.1(2) . . ?
O12 S2 O13 112.0(3) . . ?
O14 S2 O13 108.5(3) . . ?
C64 N11 C62 127.1(4) . . ?
C57 N10 C58 128.3(4) . . ?
C64 N12 C65 126.4(4) . . ?
C33 N6 C34 122.9(4) . . ?
C16 N3 C14 124.4(5) . . ?
O6 C64 N11 124.1(5) . . ?
O6 C64 N12 124.0(4) . . ?
N11 C64 N12 111.9(4) . . ?
C31 N5 C33 126.8(4) . . ?
C57 N9 C55 126.5(5) . . ?
C9 N1 C7 127.1(6) . . ?
C40 N7 C38 124.2(4) . . ?
C40 N8 C41 125.4(5) . . ?
C133 N16 C121 112.6(5) . . ?
C133 N16 C125 105.2(4) . . ?
C121 N16 C125 111.3(5) . . ?
C133 N16 C129 110.8(5) . . ?
C121 N16 C129 105.6(4) . . ?
C125 N16 C129 111.5(5) . . ?
C58 C63 C62 119.2(5) . . ?
C61 C62 C63 121.5(5) . . ?
C61 C62 N11 114.5(5) . . ?
C63 C62 N11 123.9(5) . . ?
C15 C10 C11 120.3(5) . . ?
C15 C10 N2 125.2(5) . . ?
C11 C10 N2 114.5(5) . . ?
C16 N4 C17 124.7(5) . . ?
C66 C65 C72 118.3(5) . . ?
C66 C65 N12 124.7(5) . . ?
C72 C65 N12 116.9(5) . . ?
O5 C57 N10 124.6(5) . . ?
O5 C57 N9 123.5(5) . . ?
N10 C57 N9 111.9(5) . . ?
O3 C33 N6 125.5(5) . . ?
O3 C33 N5 122.1(5) . . ?
N6 C33 N5 112.4(5) . . ?
C34 C39 C38 120.9(5) . . ?
C13 C14 C15 121.5(5) . . ?
C13 C14 N3 117.7(5) . . ?
C15 C14 N3 120.8(5) . . ?
C59 C58 C63 120.0(5) . . ?
C59 C58 N10 116.4(5) . . ?
C63 C58 N10 123.6(5) . . ?
C30 C31 N5 124.2(5) . . ?
C30 C31 C32 119.0(5) . . ?
N5 C31 C32 116.8(5) . . ?
C39 C34 C35 119.9(5) . . ?
C39 C34 N6 121.3(5) . . ?
C35 C34 N6 118.8(5) . . ?
C24 C17 C18 120.2(6) . . ?
C24 C17 N4 117.0(6) . . ?
C18 C17 N4 122.8(5) . . ?
C10 C15 C14 119.3(5) . . ?
C65 C66 C67 119.8(5) . . ?
O2 C16 N4 124.8(5) . . ?
O2 C16 N3 123.2(5) . . ?
N4 C16 N3 112.0(5) . . ?
C70 C72 C65 121.0(5) . . ?
C50 C56 C55 120.6(5) . . ?
C39 C38 N7 123.5(5) . . ?
C39 C38 C37 118.6(5) . . ?
N7 C38 C37 117.9(5) . . ?
C54 C55 N9 125.2(5) . . ?
C54 C55 C56 117.2(5) . . ?
N9 C55 C56 117.6(5) . . ?
C12 C11 C10 118.4(5) . . ?
C60 C61 C62 117.7(5) . . ?
C56 C50 C51 121.9(5) . . ?
C56 C50 C49 117.3(6) . . ?
C51 C50 C49 120.8(6) . . ?
C85 N13 C73 112.7(6) . . ?
C85 N13 C77 106.5(5) . . ?
C73 N13 C77 110.8(6) . . ?
C85 N13 C81 112.2(6) . . ?
C73 N13 C81 104.9(6) . . ?
C77 N13 C81 109.9(6) . . ?
C36 C37 C38 120.3(5) . . ?
O4 C40 N7 124.2(5) . . ?
O4 C40 N8 124.2(6) . . ?
N7 C40 N8 111.5(5) . . ?
C48 C41 C42 118.1(6) . . ?
C48 C41 N8 118.5(5) . . ?
C42 C41 N8 123.4(5) . . ?
C125 C126 C127 110.0(5) . . ?
C97 N14 C93 116.9(6) . . ?
C97 N14 C101 110.3(7) . . ?
C93 N14 C101 109.6(7) . . ?
C97 N14 C89 109.3(7) . . ?
C93 N14 C89 100.2(8) . . ?
C101 N14 C89 110.0(8) . . ?
C43 C42 C41 119.6(6) . . ?
C22 C24 C17 119.3(6) . . ?
C60 C59 C58 119.5(5) . . ?
C69 C67 C66 121.1(5) . . ?
C69 C67 C68 117.7(6) . . ?
C66 C67 C68 121.2(6) . . ?
C28 C30 C31 120.5(5) . . ?
C19 C18 C17 118.9(6) . . ?
C46 C48 C41 121.0(6) . . ?
C26 C32 C31 120.3(5) . . ?
C113 N15 C105 107.0(5) . . ?
C113 N15 C109 111.1(6) . . ?
C105 N15 C109 111.2(6) . . ?
C113 N15 C117 112.5(6) . . ?
C105 N15 C117 111.5(6) . . ?
C109 N15 C117 103.6(5) . . ?
C11 C12 C13 122.7(6) . . ?
C14 C13 C12 117.8(5) . . ?
C32 C26 C27 122.1(5) . . ?
C32 C26 C25 123.4(7) . . ?
C27 C26 C25 114.5(7) . . ?
C37 C36 C35 120.9(5) . . ?
C55 C54 C52 121.0(5) . . ?
C126 C125 N16 116.9(4) . . ?
C30 C28 C27 121.4(6) . . ?
C30 C28 C29 117.3(7) . . ?
C27 C28 C29 121.2(7) . . ?
C69 C70 C72 120.3(5) . . ?
C69 C70 C71 119.5(6) . . ?
C72 C70 C71 119.5(6) . . ?
C36 C35 C34 119.4(5) . . ?
C50 C51 C52 118.1(6) . . ?
C61 C60 C59 121.9(5) . . ?
C22 C21 C19 119.6(6) . . ?
N16 C121 C122 114.9(4) . . ?
C54 C52 C51 121.1(5) . . ?
C54 C52 C53 120.2(6) . . ?
C51 C52 C53 118.7(6) . . ?
N16 C133 C134 116.5(5) . . ?
C21 C19 C18 120.9(6) . . ?
C21 C19 C20 117.0(6) . . ?
C18 C19 C20 121.3(6) . . ?
C130 C129 N16 116.8(5) . . ?
C45 C43 C42 121.4(6) . . ?
C45 C43 C44 119.8(7) . . ?
C42 C43 C44 118.8(6) . . ?
C24 C22 C21 121.1(6) . . ?
C24 C22 C23 119.0(7) . . ?
C21 C22 C23 119.9(7) . . ?
C48 C46 C45 121.4(6) . . ?
C48 C46 C47 120.3(7) . . ?
C45 C46 C47 118.3(7) . . ?
N15 C105 C106 120.6(6) . . ?
C26 C27 C28 116.7(6) . . ?
C70 C69 C67 119.4(5) . . ?
N1 C7 C6 124.1(6) . . ?
N1 C7 C8 117.1(7) . . ?
C6 C7 C8 118.8(7) . . ?
F26 C49 F27 106.4(8) . . ?
F26 C49 F25 106.6(7) . . ?
F27 C49 F25 98.3(7) . . ?
F26 C49 C50 118.2(7) . . ?
F27 C49 C50 113.9(6) . . ?
F25 C49 C50 111.4(7) . . ?
C118 C117 N15 114.1(6) . . ?
C3 C4 C6 122.3(9) . . ?
C3 C4 C5 118.6(10) . . ?
C6 C4 C5 119.1(9) . . ?
C79 C78 C77 110.8(6) . . ?
F32 C68 F31 126.7(9) . . ?
F32 C68 F33B 79.8(9) . . ?
F31 C68 F33B 94.6(11) . . ?
F32 C68 F33A 68.1(10) . . ?
F31 C68 F33A 79.7(8) . . ?
F33B C68 F33A 133.3(7) . . ?
F32 C68 C67 115.0(9) . . ?
F31 C68 C67 115.2(6) . . ?
F33B C68 C67 114.9(8) . . ?
F33A C68 C67 109.1(9) . . ?
C7 C6 C4 118.5(7) . . ?
C8 C2 C3 120.8(8) . . ?
C8 C2 C1 113.2(13) . . ?
C3 C2 C1 126.0(14) . . ?
C97 C98 C99 115.0(7) . . ?
C80 C79 C78 114.5(7) . . ?
C123 C122 C121 111.6(5) . . ?
C74 C73 N13 115.8(6) . . ?
C128 C127 C126 115.2(6) . . ?
C46 C45 C43 118.5(6) . . ?
C2 C8 C7 120.8(8) . . ?
F28 C53 F30 106.8(9) . . ?
F28 C53 F29 103.4(8) . . ?
F30 C53 F29 105.3(7) . . ?
F28 C53 C52 113.3(7) . . ?
F30 C53 C52 115.6(7) . . ?
F29 C53 C52 111.5(8) . . ?
C114 C113 N15 116.8(7) . . ?
C78 C77 N13 116.6(5) . . ?
C129 C130 C131 110.7(6) . . ?
C98 C97 N14 120.6(7) . . ?
C115 C114 C113 108.7(9) . . ?
N13 C85 C86 115.0(6) . . ?
C110 C109 N15 120.0(7) . . ?
C73 C74 C75 106.6(6) . . ?
C124 C123 C122 114.3(7) . . ?
C98 C99 C100 116.3(9) . . ?
C4 C3 C2 118.9(9) . . ?
C87 C86 C85 111.2(8) . . ?
C130 C131 C132 114.7(7) . . ?
F7 C20 F9 129.7(16) . . ?
F7 C20 F8 89.9(11) . . ?
F9 C20 F8 93.9(10) . . ?
F7 C20 C19 114.8(8) . . ?
F9 C20 C19 114.6(9) . . ?
F8 C20 C19 96.0(12) . . ?
C120 C119 C118 112.6(9) . . ?
C119 C118 C117 108.5(7) . . ?
F11 C23 F12 100.9(8) . . ?
F11 C23 F10 104.0(9) . . ?
F12 C23 F10 103.6(11) . . ?
F11 C23 C22 116.9(10) . . ?
F12 C23 C22 112.5(9) . . ?
F10 C23 C22 116.9(7) . . ?
C111 C110 C109 107.8(8) . . ?
F21 C44 F19 110.7(8) . . ?
F21 C44 F20 104.9(8) . . ?
F19 C44 F20 99.9(7) . . ?
F21 C44 C43 116.2(8) . . ?
F19 C44 C43 113.4(7) . . ?
F20 C44 C43 110.1(7) . . ?
C112 C111 C110 101.3(10) . . ?
C76 C75 C74 109.8(7) . . ?
C102 C101 N14 125.3(12) . . ?
C114 C115 C116 111.1(10) . . ?
F4 C5 F5 111.6(15) . . ?
F4 C5 F6 99.9(13) . . ?
F5 C5 F6 103.2(10) . . ?
F4 C5 C4 115.5(10) . . ?
F5 C5 C4 115.5(12) . . ?
F6 C5 C4 109.1(14) . . ?
C94 C93 N14 111.8(10) . . ?
C93 C94 C95 110.9(9) . . ?
O1 C9 N2 126.0(6) . . ?
O1 C9 N1 123.3(6) . . ?
N2 C9 N1 110.7(6) . . ?
C9 N2 C10 126.1(5) . . ?
C96 C95 C94 110.4(9) . . ?
C86 C87 C88 109.0(11) . . ?
C105 C106 C107 112.5(7) . . ?
F18 C29 F16 109.0(14) . . ?
F18 C29 F17 102.9(13) . . ?
F16 C29 F17 99.2(9) . . ?
F18 C29 C28 119.5(7) . . ?
F16 C29 C28 112.8(11) . . ?
F17 C29 C28 111.0(14) . . ?
F15A C25 F13 81.8(11) . . ?
F15A C25 F14 127.3(10) . . ?
F13 C25 F14 99.4(12) . . ?
F15A C25 F15B 59.3(13) . . ?
F13 C25 F15B 135.2(15) . . ?
F14 C25 F15B 89.0(12) . . ?
F15A C25 C26 118.1(10) . . ?
F13 C25 C26 109.5(10) . . ?
F14 C25 C26 111.0(9) . . ?
F15B C25 C26 108.1(11) . . ?
F36 C71 F34 127.3(12) . . ?
F36 C71 F35 86.3(12) . . ?
F34 C71 F35 88.7(11) . . ?
F36 C71 C70 116.4(8) . . ?
F34 C71 C70 116.3(9) . . ?
F35 C71 C70 96.8(13) . . ?
F24 C47 F23 104.5(13) . . ?
F24 C47 F22 101.9(10) . . ?
F23 C47 F22 102.7(11) . . ?
F24 C47 C46 116.2(9) . . ?
F23 C47 C46 118.9(9) . . ?
F22 C47 C46 110.5(12) . . ?
F2 C1 F3 129(4) . . ?
F2 C1 F1 104(2) . . ?
F3 C1 F1 102(2) . . ?
F2 C1 C2 113(3) . . ?
F3 C1 C2 105.0(17) . . ?
F1 C1 C2 101(2) . . ?
C108 C107 C106 109.9(10) . . ?
C136 C135 C134 86.9(13) . . ?
C133 C134 C135 106.4(8) . . ?
C104 C103 C102 117.2(14) . . ?
C101 C102 C103 126.4(17) . . ?
C92 C91 C90 107.2(17) . . ?
C89 C90 C91 138.3(12) . . ?
C90 C89 N14 150.5(12) . . ?
N13 C81 C82 112.6(8) . . ?
C83 C82 C81 116.8(18) . . ?
C82 C83 C84 112(3) . . ?

_refine_diff_density_max         0.417
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_L-TBAOAc_H2O
_database_code_depnum_ccdc_archive 'CCDC 1551282'
_audit_update_record             
;
2017-05-20 deposited with the CCDC.
2017-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H14 F12 N4 O2, C16 H36 N, C2 H3 O2, O'
_chemical_formula_sum            'C42 H53 F12 N5 O5'
_chemical_formula_weight         935.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.4502(11)
_cell_length_b                   8.6269(15)
_cell_length_c                   20.472(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.730(8)
_cell_angle_gamma                90
_cell_volume                     2367.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2792
_cell_measurement_theta_min      3.3630
_cell_measurement_theta_max      22.8330

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_F_000             976.0
_exptl_transmission_factor_min   0.965
_exptl_transmission_factor_max   0.976
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.118
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12485
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.938
_diffrn_reflns_theta_max         28.732
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.685
_diffrn_reflns_point_group_measured_fraction_full 0.810
_reflns_number_total             11419
_reflns_number_gt                7479
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.476
_reflns_Friedel_fraction_max     0.472
_reflns_Friedel_fraction_full    0.595

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0800P)²+1.2227P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0058(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 790 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11419
_refine_ls_number_parameters     592
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2019
_refine_ls_R_factor_gt           0.1119
_refine_ls_wR_factor_ref         0.2878
_refine_ls_wR_factor_gt          0.2513
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_restrained_S_all      1.177
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.004

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
C17 C 1.2615(7) 0.8111(15) 0.7558(5) 0.064(3) Uani 1 1 d . . . . .
N3 N 1.1170(5) 0.6494(12) 0.8812(4) 0.065(3) Uani 1 1 d . . . . .
H3N H 1.1712 0.6545 0.9065 0.078 Uiso 1 1 calc R U . . .
N4 N 1.2218(5) 0.7541(12) 0.8109(4) 0.068(3) Uani 1 1 d . . . . .
H4N H 1.2635 0.7471 0.8449 0.082 Uiso 1 1 calc R U . . .
N1 N 0.6269(5) 0.4991(13) 0.8129(3) 0.071(3) Uani 1 1 d . . . . .
H1N H 0.5959 0.4992 0.8481 0.085 Uiso 1 1 calc R U . . .
O1 O 0.7787(4) 0.5446(11) 0.7750(3) 0.078(3) Uani 1 1 d . . . . .
O4 O 0.6323(5) 0.3986(11) -0.0260(3) 0.088(3) Uani 1 1 d . . . . .
O5 O 0.3302(4) 0.6832(10) 0.9317(3) 0.079(2) Uani 1 1 d . . . . .
C14 C 1.0355(6) 0.5840(14) 0.9098(4) 0.061(3) Uani 1 1 d . . . . .
O2 O 1.0567(5) 0.7121(11) 0.7782(3) 0.081(3) Uani 1 1 d . . . . .
C19 C 1.2530(8) 0.8954(16) 0.6455(5) 0.077(3) Uani 1 1 d . . . . .
O3 O 0.5078(5) 0.5329(12) -0.0785(3) 0.087(3) Uani 1 1 d . . . . .
C18 C 1.2047(7) 0.8376(15) 0.6980(5) 0.068(3) Uani 1 1 d . . . . .
H18 H 1.1365 0.8176 0.6940 0.081 Uiso 1 1 calc R U . . .
C16 C 1.1236(6) 0.7051(14) 0.8207(4) 0.056(3) Uani 1 1 d . . . . .
C15 C 0.9414(5) 0.5765(12) 0.8772(4) 0.048(2) Uani 1 1 d . . . . .
H15 H 0.9295 0.6151 0.8348 0.058 Uiso 1 1 calc R U . . .
C42 C 0.5523(8) 0.4714(17) -0.0276(6) 0.083(4) Uani 1 1 d . . . . .
N2 N 0.7643(5) 0.4988(12) 0.8851(4) 0.066(3) Uani 1 1 d . . . . .
H2N H 0.7211 0.4813 0.9129 0.079 Uiso 1 1 calc R U . . .
C24 C 1.3613(7) 0.8484(14) 0.7587(6) 0.074(3) Uani 1 1 d . . . . .
H24 H 1.3997 0.8320 0.7979 0.088 Uiso 1 1 calc R U . . .
C9 C 0.7269(5) 0.5148(14) 0.8207(4) 0.057(3) Uani 1 1 d . . . . .
C10 C 0.8626(6) 0.5073(14) 0.9105(4) 0.058(3) Uani 1 1 d . . . . .
C7 C 0.5683(6) 0.4829(14) 0.7538(4) 0.059(3) Uani 1 1 d . . . . .
F3 F 0.2619(6) 0.4383(14) 0.7547(6) 0.164(5) Uani 1 1 d . . . . .
N5 N 0.0773(6) 0.6493(14) 0.2615(4) 0.077(3) Uani 1 1 d . . . . .
C2 C 0.4069(7) 0.4261(18) 0.6999(6) 0.083(4) Uani 1 1 d . . . . .
C11 C 0.8849(6) 0.4417(16) 0.9723(4) 0.071(3) Uani 1 1 d . . . . .
H11 H 0.8357 0.3895 0.9929 0.085 Uiso 1 1 calc R U . . .
C22 C 1.4053(8) 0.9058(17) 0.7092(8) 0.091(4) Uani 1 1 d . . . . .
F8 F 1.0991(7) 0.937(2) 0.5865(4) 0.233(9) Uani 1 1 d . . . . .
C13 C 1.0549(6) 0.5223(15) 0.9720(4) 0.067(3) Uani 1 1 d . . . . .
H13 H 1.1190 0.5272 0.9928 0.080 Uiso 1 1 calc R U . . .
C12 C 0.9795(7) 0.4538(18) 1.0029(5) 0.083(4) Uani 1 1 d . . . . .
H12 H 0.9926 0.4151 1.0452 0.099 Uiso 1 1 calc R U . . .
C8 C 0.4687(6) 0.4458(15) 0.7551(5) 0.069(3) Uani 1 1 d . . . . .
H8 H 0.4428 0.4338 0.7956 0.083 Uiso 1 1 calc R U . . .
C6 C 0.6072(7) 0.4855(16) 0.6915(5) 0.075(4) Uani 1 1 d . . . . .
H6 H 0.6744 0.5064 0.6881 0.091 Uiso 1 1 calc R U . . .
F1 F 0.2432(7) 0.458(2) 0.6595(7) 0.223(7) Uani 1 1 d . . . . .
C37 C 0.1027(7) 0.5281(19) 0.3130(6) 0.093(4) Uani 1 1 d . . . . .
H37A H 0.1064 0.4284 0.2913 0.111 Uiso 1 1 calc R U . . .
H37B H 0.0484 0.5226 0.3413 0.111 Uiso 1 1 calc R U . . .
F2 F 0.2790(8) 0.2470(16) 0.6947(12) 0.296(14) Uani 1 1 d . . . . .
C27 C 0.2444(9) 0.5406(19) 0.1229(6) 0.092(4) Uani 1 1 d . . . . .
H27A H 0.2130 0.6148 0.0921 0.110 Uiso 1 1 calc R U . . .
H27B H 0.3057 0.5864 0.1424 0.110 Uiso 1 1 calc R U . . .
C4 C 0.5446(9) 0.457(2) 0.6363(5) 0.097(5) Uani 1 1 d . . . . .
C25 C 0.1574(8) 0.6622(18) 0.2137(6) 0.085(4) Uani 1 1 d . . . . .
H25A H 0.2198 0.6932 0.2373 0.102 Uiso 1 1 calc R U . . .
H25B H 0.1387 0.7418 0.1816 0.102 Uiso 1 1 calc R U . . .
C30 C -0.0671(8) 0.7075(18) 0.1733(7) 0.094(4) Uani 1 1 d . . . . .
H30A H -0.0189 0.7142 0.1407 0.113 Uiso 1 1 calc R U . . .
H30B H -0.0814 0.8118 0.1876 0.113 Uiso 1 1 calc R U . . .
C29 C -0.0248(8) 0.6139(18) 0.2305(6) 0.093(5) Uani 1 1 d . . . . .
H29A H -0.0249 0.5063 0.2167 0.112 Uiso 1 1 calc R U . . .
H29B H -0.0707 0.6219 0.2644 0.112 Uiso 1 1 calc R U . . .
C21 C 1.3519(9) 0.9279(17) 0.6489(7) 0.094(4) Uani 1 1 d . . . . .
H21 H 1.3825 0.9633 0.6126 0.113 Uiso 1 1 calc R U . . .
C28 C 0.2672(11) 0.402(2) 0.0887(8) 0.135(6) Uani 1 1 d . . . . .
H28A H 0.2891 0.3234 0.1197 0.202 Uiso 1 1 calc R U . . .
H28B H 0.3192 0.4232 0.0605 0.202 Uiso 1 1 calc R U . . .
H28C H 0.2087 0.3670 0.0629 0.202 Uiso 1 1 calc R U . . .
C33 C 0.0754(8) 0.8082(19) 0.2932(6) 0.093(4) Uani 1 1 d . . . . .
H33A H 0.0579 0.8831 0.2588 0.112 Uiso 1 1 calc R U . . .
H33B H 0.1427 0.8320 0.3110 0.112 Uiso 1 1 calc R U . . .
C31 C -0.1648(9) 0.6299(18) 0.1427(6) 0.095(4) Uani 1 1 d . . . . .
H31A H -0.1492 0.5293 0.1250 0.113 Uiso 1 1 calc R U . . .
H31B H -0.2102 0.6141 0.1765 0.113 Uiso 1 1 calc R U . . .
C3 C 0.4439(8) 0.4253(18) 0.6379(6) 0.094(4) Uani 1 1 d . . . . .
H3 H 0.4031 0.4046 0.6000 0.113 Uiso 1 1 calc R U . . .
C34 C 0.0052(9) 0.835(3) 0.3481(7) 0.128(7) Uani 1 1 d . . . . .
H34A H -0.0636 0.8281 0.3302 0.153 Uiso 1 1 calc R U . . .
H34B H 0.0164 0.7552 0.3814 0.153 Uiso 1 1 calc R U . . .
C20 C 1.1864(12) 0.917(3) 0.5834(7) 0.118(6) Uani 1 1 d . . . . .
F9 F 1.1984(9) 0.823(2) 0.5398(6) 0.189(6) Uani 1 1 d . . . . .
C26 C 0.1728(9) 0.506(2) 0.1779(6) 0.113(6) Uani 1 1 d . . . . .
H26A H 0.1094 0.4662 0.1588 0.135 Uiso 1 1 calc R U . . .
H26B H 0.2023 0.4293 0.2084 0.135 Uiso 1 1 calc R U . . .
C38 C 0.2013(9) 0.553(2) 0.3566(7) 0.126(6) Uani 1 1 d . . . . .
H38B H 0.1994 0.6497 0.3808 0.151 Uiso 1 1 calc R U . . .
H38A H 0.2580 0.5552 0.3302 0.151 Uiso 1 1 calc R U . . .
C5 C 0.5897(16) 0.485(6) 0.5703(8) 0.198(17) Uani 1 1 d . . . . .
C41 C 0.5139(11) 0.500(3) 0.0380(6) 0.173(11) Uani 1 1 d . . . . .
H41A H 0.4462 0.4641 0.0375 0.260 Uiso 1 1 calc R U . . .
H41B H 0.5163 0.6088 0.0476 0.260 Uiso 1 1 calc R U . . .
H41C H 0.5545 0.4447 0.0711 0.260 Uiso 1 1 calc R U . . .
F6B F 0.652(3) 0.562(7) 0.5712(17) 0.26(3) Uani 0.5 1 d . . P . .
F4 F 0.5426(14) 0.519(6) 0.5288(10) 0.37(2) Uani 1 1 d . . . . .
C32 C -0.2140(12) 0.728(3) 0.0898(8) 0.161(8) Uani 1 1 d . . . . .
H32A H -0.2268 0.8287 0.1068 0.241 Uiso 1 1 calc R U . . .
H32B H -0.2758 0.6806 0.0735 0.241 Uiso 1 1 calc R U . . .
H32C H -0.1711 0.7369 0.0548 0.241 Uiso 1 1 calc R U . . .
F7 F 1.2207(11) 1.048(2) 0.5513(6) 0.211(7) Uani 1 1 d . . . . .
F5 F 0.588(3) 0.347(3) 0.5444(13) 0.332(18) Uani 1 1 d . . . . .
C35 C 0.0248(16) 0.994(3) 0.3788(9) 0.168(9) Uani 1 1 d . . . . .
H35A H 0.0948 1.0008 0.3943 0.202 Uiso 1 1 calc R U . . .
H35B H 0.0117 1.0722 0.3453 0.202 Uiso 1 1 calc R U . . .
F6A F 0.6900(18) 0.447(7) 0.5750(11) 0.24(3) Uani 0.5 1 d . . P . .
C39 C 0.2075(13) 0.409(3) 0.4049(8) 0.183(10) Uani 1 1 d . . . . .
H39A H 0.2173 0.3143 0.3806 0.219 Uiso 1 1 calc R U . . .
H39B H 0.1459 0.3994 0.4261 0.219 Uiso 1 1 calc R U . . .
C40 C 0.2995(17) 0.435(4) 0.4587(10) 0.221(12) Uani 1 1 d . . . . .
H40C H 0.3298 0.3372 0.4703 0.332 Uiso 1 1 calc R U . . .
H40B H 0.2759 0.4823 0.4970 0.332 Uiso 1 1 calc R U . . .
H40A H 0.3478 0.5018 0.4411 0.332 Uiso 1 1 calc R U . . .
C36 C -0.0376(18) 1.029(4) 0.4354(10) 0.254(19) Uani 1 1 d . . . . .
H36A H -0.1031 0.9859 0.4264 0.381 Uiso 1 1 calc R U . . .
H36B H -0.0426 1.1391 0.4408 0.381 Uiso 1 1 calc R U . . .
H36C H -0.0067 0.9838 0.4749 0.381 Uiso 1 1 calc R U . . .
C1 C 0.2998(9) 0.373(3) 0.7044(11) 0.138(7) Uani 1 1 d . . . . .
F12 F 1.5523(10) 0.947(6) 0.6690(10) 0.45(3) Uani 1 1 d . . . . .
F11 F 1.5296(11) 1.082(2) 0.723(2) 0.39(2) Uani 1 1 d . . . . .
C23 C 1.5126(12) 0.952(3) 0.7186(13) 0.152(8) Uani 1 1 d . . . . .
F10 F 1.5656(8) 0.8666(19) 0.7543(10) 0.234(9) 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
C17 C18 1.374(14) . ?
C17 N4 1.378(13) . ?
C17 C24 1.378(13) . ?
N3 C16 1.338(11) . ?
N3 C14 1.403(12) . ?
N4 C16 1.416(11) . ?
N1 C9 1.349(10) . ?
N1 C7 1.396(11) . ?
O1 C9 1.239(10) . ?
O4 C42 1.244(13) . ?
C14 C15 1.382(11) . ?
C14 C13 1.386(13) . ?
O2 C16 1.201(10) . ?
C19 C21 1.356(15) . ?
C19 C18 1.392(14) . ?
C19 C20 1.507(19) . ?
O3 C42 1.275(13) . ?
C15 C10 1.438(12) . ?
C42 C41 1.499(15) . ?
N2 C9 1.378(11) . ?
N2 C10 1.382(10) . ?
C24 C22 1.311(16) . ?
C10 C11 1.396(13) . ?
C7 C8 1.379(12) . ?
C7 C6 1.417(12) . ?
F3 C1 1.315(19) . ?
N5 C29 1.496(13) . ?
N5 C37 1.504(15) . ?
N5 C25 1.517(13) . ?
N5 C33 1.518(17) . ?
C2 C8 1.356(14) . ?
C2 C3 1.401(15) . ?
C2 C1 1.522(19) . ?
C11 C12 1.375(12) . ?
C22 C21 1.389(17) . ?
C22 C23 1.493(19) . ?
F8 C20 1.193(15) . ?
C13 C12 1.373(13) . ?
C6 C4 1.377(14) . ?
F1 C1 1.36(2) . ?
C37 C38 1.552(16) . ?
F2 C1 1.13(2) . ?
C27 C28 1.43(2) . ?
C27 C26 1.570(16) . ?
C4 C3 1.384(15) . ?
C4 C5 1.54(2) . ?
C25 C26 1.56(2) . ?
C30 C29 1.495(16) . ?
C30 C31 1.560(16) . ?
C33 C34 1.544(17) . ?
C31 C32 1.485(19) . ?
C34 C35 1.52(3) . ?
C20 F9 1.227(19) . ?
C20 F7 1.40(2) . ?
C38 C39 1.59(2) . ?
C5 F4 1.06(3) . ?
C5 F6B 1.06(4) . ?
C5 F5 1.30(4) . ?
C5 F6A 1.38(4) . ?
C35 C36 1.52(2) . ?
C39 C40 1.60(2) . ?
F12 C23 1.19(2) . ?
F11 C23 1.14(3) . ?
C23 F10 1.22(2) . ?

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
C18 C17 N4 122.6(8) . . ?
C18 C17 C24 117.9(10) . . ?
N4 C17 C24 119.4(9) . . ?
C16 N3 C14 130.1(7) . . ?
C17 N4 C16 130.7(8) . . ?
C9 N1 C7 126.8(7) . . ?
C15 C14 C13 121.4(8) . . ?
C15 C14 N3 122.2(8) . . ?
C13 C14 N3 116.3(8) . . ?
C21 C19 C18 123.6(11) . . ?
C21 C19 C20 122.0(12) . . ?
C18 C19 C20 114.4(11) . . ?
C17 C18 C19 117.5(10) . . ?
O2 C16 N3 125.9(8) . . ?
O2 C16 N4 122.2(9) . . ?
N3 C16 N4 111.9(7) . . ?
C14 C15 C10 118.2(8) . . ?
O4 C42 O3 125.3(10) . . ?
O4 C42 C41 114.9(11) . . ?
O3 C42 C41 119.5(11) . . ?
C9 N2 C10 128.2(7) . . ?
C22 C24 C17 123.8(11) . . ?
O1 C9 N1 123.3(8) . . ?
O1 C9 N2 124.0(7) . . ?
N1 C9 N2 112.6(7) . . ?
N2 C10 C11 116.6(8) . . ?
N2 C10 C15 124.3(8) . . ?
C11 C10 C15 119.1(7) . . ?
C8 C7 N1 119.1(8) . . ?
C8 C7 C6 116.9(9) . . ?
N1 C7 C6 123.7(8) . . ?
C29 N5 C37 107.6(9) . . ?
C29 N5 C25 114.6(9) . . ?
C37 N5 C25 111.7(9) . . ?
C29 N5 C33 108.6(10) . . ?
C37 N5 C33 109.8(10) . . ?
C25 N5 C33 104.3(9) . . ?
C8 C2 C3 121.1(9) . . ?
C8 C2 C1 120.4(12) . . ?
C3 C2 C1 117.5(12) . . ?
C12 C11 C10 120.3(9) . . ?
C24 C22 C21 120.3(10) . . ?
C24 C22 C23 119.6(15) . . ?
C21 C22 C23 120.1(14) . . ?
C12 C13 C14 119.9(8) . . ?
C11 C12 C13 120.9(9) . . ?
C2 C8 C7 122.8(9) . . ?
C4 C6 C7 119.3(9) . . ?
N5 C37 C38 116.1(11) . . ?
C28 C27 C26 111.1(14) . . ?
C6 C4 C3 123.3(10) . . ?
C6 C4 C5 115.6(12) . . ?
C3 C4 C5 120.6(11) . . ?
N5 C25 C26 111.6(11) . . ?
C29 C30 C31 109.7(11) . . ?
C30 C29 N5 119.9(10) . . ?
C19 C21 C22 116.8(11) . . ?
N5 C33 C34 118.6(12) . . ?
C32 C31 C30 111.0(12) . . ?
C4 C3 C2 116.3(10) . . ?
C35 C34 C33 109.8(14) . . ?
F8 C20 F9 108.8(19) . . ?
F8 C20 F7 106.0(19) . . ?
F9 C20 F7 97.1(11) . . ?
F8 C20 C19 119.4(10) . . ?
F9 C20 C19 115.2(17) . . ?
F7 C20 C19 107.5(15) . . ?
C25 C26 C27 106.6(12) . . ?
C37 C38 C39 104.3(13) . . ?
F4 C5 F6B 105(6) . . ?
F4 C5 F5 87(3) . . ?
F6B C5 F5 124(4) . . ?
F4 C5 F6A 130(2) . . ?
F6B C5 F6A 52(4) . . ?
F5 C5 F6A 78(3) . . ?
F4 C5 C4 120(2) . . ?
F6B C5 C4 116(2) . . ?
F5 C5 C4 103(3) . . ?
F6A C5 C4 111(2) . . ?
C36 C35 C34 114(2) . . ?
C38 C39 C40 108.4(17) . . ?
F2 C1 F3 116(2) . . ?
F2 C1 F1 106.4(19) . . ?
F3 C1 F1 93.7(14) . . ?
F2 C1 C2 120.0(15) . . ?
F3 C1 C2 110.3(15) . . ?
F1 C1 C2 106.1(18) . . ?
F11 C23 F12 90(2) . . ?
F11 C23 F10 116(3) . . ?
F12 C23 F10 102(3) . . ?
F11 C23 C22 117(2) . . ?
F12 C23 C22 112(2) . . ?
F10 C23 C22 115.2(17) . . ?

_refine_diff_density_max         0.342
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.076

