# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tcnotfa4
_audit_block_doi                 10.5517/ccdc.csd.cc1phw24
_database_code_depnum_ccdc_archive 'CCDC 1564386'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT03084C 2017
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;


# start Validation Reply Form

_vrf_PLAT342_tcnotfa4            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.023 Ang.  
RESPONSE: This is due to the data quality
;
_vrf_PLAT910_tcnotfa4            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          16 Note  
RESPONSE: This is due to the data quality
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 F13 N O9 Tc, Cs, C16 H36 N'
_chemical_formula_sum            'C24 H36 Cs F13 N2 O9 Tc'
_chemical_formula_weight         974.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 '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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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                   14.7160(10)
_cell_length_b                   9.6050(10)
_cell_length_c                   28.907(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.870(10)
_cell_angle_gamma                90
_cell_volume                     3736.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6422
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      27.43

_exptl_crystal_description       plate
_exptl_crystal_colour            pale-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_F_000             1924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.456
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            15306
_diffrn_reflns_av_unetI/netI     0.1519
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.325
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6539
_reflns_number_gt                3098
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    Ortep
_computing_publication_material  WingX
_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)+(0.0263P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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         6539
_refine_ls_number_parameters     455
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.0967
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_restrained_S_all      0.865
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc2 Tc 0.02705(5) 0.84579(6) 0.83450(3) 0.0427(2) Uani 1 1 d . . . . .
O5 O 0.1306(4) 0.6983(5) 0.8720(2) 0.0545(15) Uani 1 1 d . . . . .
O4 O -0.0726(4) 0.7076(5) 0.8427(2) 0.0537(15) Uani 1 1 d . . . . .
F1 F 0.0085(3) 0.7292(4) 0.77459(16) 0.0490(11) Uani 1 1 d . . . . .
O1 O 0.0572(5) 1.0053(6) 0.9252(3) 0.0751(19) Uani 1 1 d . . . . .
N1 N 0.0444(5) 0.9434(7) 0.8882(3) 0.0577(19) Uani 1 1 d . . . . .
Cs1 Cs 0.01343(4) 0.42610(5) 0.80845(2) 0.05404(18) Uani 1 1 d . . . . .
O8 O 0.2403(5) 0.8162(7) 0.9370(3) 0.112(3) Uani 1 1 d . . . . .
F63 F 0.3543(6) 0.5924(9) 0.9547(5) 0.198(5) Uani 1 1 d . . . . .
C5 C 0.2069(7) 0.7123(10) 0.9126(4) 0.062(3) Uani 1 1 d . . . . .
O9 O -0.1564(5) 0.8503(8) 0.8716(3) 0.107(3) Uani 1 1 d . . . . .
C6 C 0.2598(8) 0.5779(14) 0.9301(5) 0.086(3) Uani 1 1 d . . . . .
F83 F -0.1757(6) 0.4949(8) 0.8485(4) 0.158(4) Uani 1 1 d . . . . .
F81 F -0.2172(7) 0.6090(9) 0.9002(3) 0.171(4) Uani 1 1 d . . . . .
F82 F -0.2935(6) 0.6303(10) 0.8239(4) 0.178(4) Uani 1 1 d . . . . .
C8 C -0.2023(9) 0.6136(14) 0.8577(6) 0.094(4) Uani 1 1 d . . . . .
C7 C -0.1381(7) 0.7387(11) 0.8581(4) 0.070(3) Uani 1 1 d . . . . .
F62 F 0.2420(9) 0.5250(10) 0.9670(5) 0.218(6) Uani 1 1 d . . . . .
F61 F 0.2491(7) 0.4830(8) 0.8999(3) 0.181(5) Uani 1 1 d . . . . .
O2 O -0.0860(3) 0.9588(5) 0.78424(19) 0.0490(14) Uani 1 1 d . . . . .
O3 O 0.1256(3) 0.9500(5) 0.8149(2) 0.0533(15) Uani 1 1 d . . . . .
O7 O 0.1435(5) 1.1548(7) 0.8570(3) 0.080(2) Uani 1 1 d . . . . .
O6 O -0.0927(4) 1.1504(7) 0.8271(3) 0.077(2) Uani 1 1 d . . . . .
C1 C -0.1236(6) 1.0727(10) 0.7915(4) 0.052(2) Uani 1 1 d . . . . .
C3 C 0.1627(6) 1.0721(11) 0.8318(4) 0.063(2) Uani 1 1 d . . . . .
F42 F 0.2267(5) 1.0706(8) 0.7678(3) 0.120(2) Uani 1 1 d . . . . .
F21 F -0.2223(4) 1.0747(9) 0.7031(3) 0.117(2) Uani 1 1 d . . . . .
F22 F -0.2937(4) 1.0645(11) 0.7516(3) 0.176(4) Uani 1 1 d . . . . .
F23 F -0.2306(6) 1.2458(8) 0.7415(3) 0.150(3) Uani 1 1 d . . . . .
F41 F 0.3282(5) 1.0450(12) 0.8420(4) 0.191(5) Uani 1 1 d . . . . .
C2 C -0.2178(8) 1.1116(11) 0.7471(5) 0.076(3) Uani 1 1 d . . . . .
F43 F 0.2637(8) 1.2394(9) 0.8161(5) 0.206(5) Uani 1 1 d . . . . .
C4 C 0.2471(10) 1.1058(14) 0.8146(6) 0.100(4) Uani 1 1 d . . . . .
N2 N -0.3125(8) 1.1126(9) 0.9130(4) 0.102(3) Uani 1 1 d . U . . .
C11 C -0.3409(12) 1.0670(19) 0.8602(6) 0.182(7) Uani 1 1 d D U . . .
H11A H -0.3509 1.1477 0.8386 0.218 Uiso 1 1 calc R U . . .
H11B H -0.2878 1.0115 0.8579 0.218 Uiso 1 1 calc R U . . .
C12 C -0.4316(11) 0.9852(18) 0.8433(5) 0.166(6) Uani 1 1 d D U . . .
H12A H -0.4836 1.0386 0.8477 0.199 Uiso 1 1 calc R U . . .
H12B H -0.4203 0.9014 0.8636 0.199 Uiso 1 1 calc R U . . .
C13 C -0.4640(12) 0.9466(19) 0.7887(6) 0.187(7) Uani 1 1 d D U . . .
H13A H -0.4811 1.0316 0.7689 0.224 Uiso 1 1 calc R U . . .
H13B H -0.4076 0.9057 0.7844 0.224 Uiso 1 1 calc R U . . .
C14 C -0.5457(14) 0.853(2) 0.7678(7) 0.254(11) Uani 1 1 d D U . . .
H14A H -0.5264 0.7744 0.7533 0.381 Uiso 1 1 calc R U . . .
H14B H -0.6006 0.8996 0.7421 0.381 Uiso 1 1 calc R U . . .
H14C H -0.5651 0.8215 0.7940 0.381 Uiso 1 1 calc R U . . .
C21 C -0.2063(12) 1.1711(17) 0.9198(7) 0.159(6) Uani 1 1 d . U . . .
H21A H -0.1723 1.0947 0.9116 0.191 Uiso 1 1 calc R U . . .
H21B H -0.2188 1.2405 0.8935 0.191 Uiso 1 1 calc R U . . .
C22 C -0.1378(13) 1.2301(17) 0.9643(7) 0.179(7) Uani 1 1 d D U . . .
H22A H -0.1526 1.1828 0.9901 0.215 Uiso 1 1 calc R U . A 1
H22B H -0.1635 1.3237 0.9631 0.215 Uiso 1 1 calc R U . A 1
C23 C -0.0185(12) 1.2537(19) 0.9922(8) 0.196(7) Uani 1 1 d D U . B 1
H23A H 0.0004 1.3195 1.0200 0.235 Uiso 1 1 calc R U . B 1
H23B H 0.0183 1.1674 1.0033 0.235 Uiso 1 1 calc R U . B 1
C24 C -0.0120(17) 1.312(3) 0.9470(9) 0.306(14) Uani 1 1 d D U . B 1
H24A H -0.0494 1.2546 0.9183 0.459 Uiso 1 1 calc R U . B 1
H24B H 0.0563 1.3141 0.9515 0.459 Uiso 1 1 calc R U . B 1
H24C H -0.0385 1.4044 0.9415 0.459 Uiso 1 1 calc R U . B 1
C31 C -0.3757(9) 1.2224(11) 0.9222(4) 0.104(4) Uani 1 1 d . U . . .
H31A H -0.4392 1.1808 0.9170 0.125 Uiso 1 1 calc R U . . .
H31B H -0.3442 1.2499 0.9574 0.125 Uiso 1 1 calc R U . . .
C32 C -0.3948(9) 1.3469(13) 0.8916(5) 0.124(4) Uani 1 1 d . U . . .
H32A H -0.4201 1.3205 0.8562 0.149 Uiso 1 1 calc R U . . .
H32B H -0.3327 1.3962 0.8997 0.149 Uiso 1 1 calc R U . . .
C33 C -0.4698(11) 1.4457(15) 0.8995(6) 0.146(5) Uani 1 1 d . U . . .
H33A H -0.5318 1.3956 0.8905 0.175 Uiso 1 1 calc R U . . .
H33B H -0.4451 1.4670 0.9353 0.175 Uiso 1 1 calc R U . . .
C34 C -0.4907(9) 1.5719(15) 0.8729(6) 0.155(5) Uani 1 1 d . U . . .
H34A H -0.4326 1.6299 0.8852 0.233 Uiso 1 1 calc R U . . .
H34B H -0.5439 1.6184 0.8778 0.233 Uiso 1 1 calc R U . . .
H34C H -0.5100 1.5540 0.8375 0.233 Uiso 1 1 calc R U . . .
C41 C -0.2930(11) 0.9954(14) 0.9507(5) 0.135(5) Uani 1 1 d . U . . .
H41A H -0.2723 0.9161 0.9366 0.162 Uiso 1 1 calc R U . . .
H41B H -0.2357 1.0231 0.9806 0.162 Uiso 1 1 calc R U . . .
C42 C -0.3636(12) 0.9452(15) 0.9677(6) 0.153(5) Uani 1 1 d . U . . .
H42A H -0.4214 0.9131 0.9388 0.183 Uiso 1 1 calc R U . . .
H42B H -0.3846 1.0212 0.9832 0.183 Uiso 1 1 calc R U . . .
C43 C -0.3260(11) 0.8283(13) 1.0052(6) 0.141(5) Uani 1 1 d . U . . .
H43A H -0.3088 0.7489 0.9896 0.169 Uiso 1 1 calc R U . . .
H43B H -0.2669 0.8577 1.0340 0.169 Uiso 1 1 calc R U . . .
C44 C -0.4067(13) 0.7886(16) 1.0224(7) 0.184(7) Uani 1 1 d . U . . .
H44A H -0.4372 0.8714 1.0281 0.276 Uiso 1 1 calc R U . . .
H44B H -0.3783 0.7361 1.0532 0.276 Uiso 1 1 calc R U . . .
H44C H -0.4558 0.7332 0.9967 0.276 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
Tc2 N1 1.742(8) . ?
Tc2 F1 1.986(4) . ?
Tc2 O3 2.023(5) . ?
Tc2 O2 2.025(5) . ?
Tc2 O5 2.041(5) . ?
Tc2 O4 2.061(5) . ?
Tc2 Cs1 4.0043(10) 2_556 ?
Tc2 Cs1 4.0909(9) . ?
O5 C5 1.261(10) . ?
O5 Cs1 3.259(5) . ?
O4 C7 1.251(11) . ?
O4 Cs1 3.303(5) . ?
F1 Cs1 2.969(4) 2_556 ?
F1 Cs1 3.063(4) . ?
O1 N1 1.169(8) . ?
Cs1 F1 2.969(4) 2_546 ?
Cs1 O7 3.202(7) 1_545 ?
Cs1 O6 3.229(7) 1_545 ?
Cs1 O2 3.277(5) 2_546 ?
Cs1 O3 3.324(5) 2_546 ?
Cs1 F61 3.449(8) . ?
Cs1 F83 3.483(7) . ?
Cs1 F21 3.525(7) 2_546 ?
Cs1 F42 3.601(7) 2_546 ?
O8 C5 1.206(10) . ?
F63 C6 1.288(12) . ?
C5 C6 1.487(13) . ?
O9 C7 1.208(11) . ?
C6 F61 1.229(12) . ?
C6 F62 1.301(14) . ?
F83 C8 1.269(13) . ?
F81 C8 1.332(13) . ?
F82 C8 1.312(13) . ?
C8 C7 1.526(14) . ?
O2 C1 1.281(10) . ?
O2 Cs1 3.277(5) 2_556 ?
O3 C3 1.302(10) . ?
O3 Cs1 3.324(5) 2_556 ?
O7 C3 1.188(11) . ?
O7 Cs1 3.202(7) 1_565 ?
O6 C1 1.201(10) . ?
O6 Cs1 3.229(7) 1_565 ?
C1 C2 1.507(13) . ?
C1 Cs1 3.877(9) 1_565 ?
C3 C4 1.547(14) . ?
F42 C4 1.306(13) . ?
F42 Cs1 3.601(7) 2_556 ?
F21 C2 1.297(12) . ?
F21 Cs1 3.525(7) 2_556 ?
F22 C2 1.259(11) . ?
F23 C2 1.303(11) . ?
F23 Cs1 3.744(8) 1_565 ?
F41 C4 1.275(15) . ?
F43 C4 1.304(13) . ?
N2 C11 1.477(16) . ?
N2 C31 1.499(13) . ?
N2 C41 1.510(15) . ?
N2 C21 1.597(17) . ?
C11 C12 1.453(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.500(19) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.425(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C21 C22 1.39(2) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.625(15) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.459(10) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C31 C32 1.445(14) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.541(16) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.401(15) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C41 C42 1.403(17) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.501(17) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.510(18) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Tc2 F1 178.2(2) . . ?
N1 Tc2 O3 96.9(3) . . ?
F1 Tc2 O3 84.03(19) . . ?
N1 Tc2 O2 97.6(3) . . ?
F1 Tc2 O2 83.89(19) . . ?
O3 Tc2 O2 90.46(19) . . ?
N1 Tc2 O5 95.3(3) . . ?
F1 Tc2 O5 83.20(19) . . ?
O3 Tc2 O5 91.5(2) . . ?
O2 Tc2 O5 166.7(2) . . ?
N1 Tc2 O4 95.7(3) . . ?
F1 Tc2 O4 83.3(2) . . ?
O3 Tc2 O4 167.1(2) . . ?
O2 Tc2 O4 90.6(2) . . ?
O5 Tc2 O4 84.6(2) . . ?
N1 Tc2 Cs1 136.3(2) . 2_556 ?
F1 Tc2 Cs1 45.43(12) . 2_556 ?
O3 Tc2 Cs1 55.94(15) . 2_556 ?
O2 Tc2 Cs1 54.58(15) . 2_556 ?
O5 Tc2 Cs1 116.69(17) . 2_556 ?
O4 Tc2 Cs1 115.25(16) . 2_556 ?
N1 Tc2 Cs1 132.3(2) . . ?
F1 Tc2 Cs1 45.95(12) . . ?
O3 Tc2 Cs1 115.05(15) . . ?
O2 Tc2 Cs1 115.56(14) . . ?
O5 Tc2 Cs1 52.00(15) . . ?
O4 Tc2 Cs1 53.31(15) . . ?
Cs1 Tc2 Cs1 91.380(17) 2_556 . ?
C5 O5 Tc2 127.8(5) . . ?
C5 O5 Cs1 132.8(5) . . ?
Tc2 O5 Cs1 98.43(19) . . ?
C7 O4 Tc2 125.0(6) . . ?
C7 O4 Cs1 138.3(6) . . ?
Tc2 O4 Cs1 96.66(19) . . ?
Tc2 F1 Cs1 106.11(15) . 2_556 ?
Tc2 F1 Cs1 106.26(16) . . ?
Cs1 F1 Cs1 147.62(15) 2_556 . ?
O1 N1 Tc2 177.9(7) . . ?
F1 Cs1 F1 111.48(5) 2_546 . ?
F1 Cs1 O7 71.73(15) 2_546 1_545 ?
F1 Cs1 O7 147.84(13) . 1_545 ?
F1 Cs1 O6 73.20(15) 2_546 1_545 ?
F1 Cs1 O6 151.94(13) . 1_545 ?
O7 Cs1 O6 60.18(15) 1_545 1_545 ?
F1 Cs1 O5 145.73(13) 2_546 . ?
F1 Cs1 O5 49.93(12) . . ?
O7 Cs1 O5 108.66(14) 1_545 . ?
O6 Cs1 O5 138.18(17) 1_545 . ?
F1 Cs1 O2 50.56(11) 2_546 2_546 ?
F1 Cs1 O2 67.72(11) . 2_546 ?
O7 Cs1 O2 95.87(15) 1_545 2_546 ?
O6 Cs1 O2 123.72(16) 1_545 2_546 ?
O5 Cs1 O2 96.37(13) . 2_546 ?
F1 Cs1 O4 146.53(12) 2_546 . ?
F1 Cs1 O4 49.84(12) . . ?
O7 Cs1 O4 140.22(16) 1_545 . ?
O6 Cs1 O4 110.58(14) 1_545 . ?
O5 Cs1 O4 49.74(13) . . ?
O2 Cs1 O4 117.24(13) 2_546 . ?
F1 Cs1 O3 50.09(12) 2_546 2_546 ?
F1 Cs1 O3 70.53(12) . 2_546 ?
O7 Cs1 O3 121.74(16) 1_545 2_546 ?
O6 Cs1 O3 96.11(15) 1_545 2_546 ?
O5 Cs1 O3 120.32(13) . 2_546 ?
O2 Cs1 O3 51.61(12) 2_546 2_546 ?
O4 Cs1 O3 96.92(13) . 2_546 ?
F1 Cs1 F61 117.83(16) 2_546 . ?
F1 Cs1 F61 88.90(16) . . ?
O7 Cs1 F61 63.61(16) 1_545 . ?
O6 Cs1 F61 113.98(19) 1_545 . ?
O5 Cs1 F61 45.77(14) . . ?
O2 Cs1 F61 93.0(2) 2_546 . ?
O4 Cs1 F61 91.69(15) . . ?
O3 Cs1 F61 143.4(2) 2_546 . ?
F1 Cs1 F83 123.35(17) 2_546 . ?
F1 Cs1 F83 90.41(14) . . ?
O7 Cs1 F83 115.12(19) 1_545 . ?
O6 Cs1 F83 66.07(16) 1_545 . ?
O5 Cs1 F83 88.38(17) . . ?
O2 Cs1 F83 145.34(18) 2_546 . ?
O4 Cs1 F83 44.79(15) . . ?
O3 Cs1 F83 96.65(19) 2_546 . ?
F61 Cs1 F83 114.0(2) . . ?
F1 Cs1 F21 89.71(15) 2_546 2_546 ?
F1 Cs1 F21 59.59(16) . 2_546 ?
O7 Cs1 F21 88.96(17) 1_545 2_546 ?
O6 Cs1 F21 147.90(17) 1_545 2_546 ?
O5 Cs1 F21 56.35(16) . 2_546 ?
O2 Cs1 F21 45.45(14) 2_546 2_546 ?
O4 Cs1 F21 98.72(16) . 2_546 ?
O3 Cs1 F21 93.01(14) 2_546 2_546 ?
F61 Cs1 F21 50.4(2) . 2_546 ?
F83 Cs1 F21 143.07(18) . 2_546 ?
F1 Cs1 F42 89.52(15) 2_546 2_546 ?
F1 Cs1 F42 63.10(15) . 2_546 ?
O7 Cs1 F42 147.82(18) 1_545 2_546 ?
O6 Cs1 F42 89.84(17) 1_545 2_546 ?
O5 Cs1 F42 101.54(16) . 2_546 ?
O2 Cs1 F42 91.50(15) 2_546 2_546 ?
O4 Cs1 F42 57.84(16) . 2_546 ?
O3 Cs1 F42 44.84(15) 2_546 2_546 ?
F61 Cs1 F42 147.31(18) . 2_546 ?
F83 Cs1 F42 54.0(2) . 2_546 ?
F21 Cs1 F42 117.60(18) 2_546 2_546 ?
O8 C5 O5 129.2(8) . . ?
O8 C5 C6 119.1(9) . . ?
O5 C5 C6 111.8(9) . . ?
F61 C6 F63 105.7(11) . . ?
F61 C6 F62 106.5(14) . . ?
F63 C6 F62 97.0(10) . . ?
F61 C6 C5 120.2(9) . . ?
F63 C6 C5 113.2(12) . . ?
F62 C6 C5 111.5(11) . . ?
C8 F83 Cs1 126.6(6) . . ?
F83 C8 F82 105.2(13) . . ?
F83 C8 F81 110.1(12) . . ?
F82 C8 F81 101.0(9) . . ?
F83 C8 C7 117.8(9) . . ?
F82 C8 C7 110.7(11) . . ?
F81 C8 C7 110.6(11) . . ?
O9 C7 O4 129.2(9) . . ?
O9 C7 C8 118.8(10) . . ?
O4 C7 C8 111.9(9) . . ?
C6 F61 Cs1 117.5(7) . . ?
C1 O2 Tc2 128.6(5) . . ?
C1 O2 Cs1 121.5(5) . 2_556 ?
Tc2 O2 Cs1 95.17(18) . 2_556 ?
C3 O3 Tc2 125.5(6) . . ?
C3 O3 Cs1 116.5(5) . 2_556 ?
Tc2 O3 Cs1 93.79(17) . 2_556 ?
C3 O7 Cs1 121.5(7) . 1_565 ?
C1 O6 Cs1 114.1(6) . 1_565 ?
O6 C1 O2 129.2(8) . . ?
O6 C1 C2 118.4(9) . . ?
O2 C1 C2 112.4(9) . . ?
O6 C1 Cs1 49.5(5) . 1_565 ?
O2 C1 Cs1 122.1(5) . 1_565 ?
C2 C1 Cs1 98.2(6) . 1_565 ?
O7 C3 O3 131.6(9) . . ?
O7 C3 C4 118.6(9) . . ?
O3 C3 C4 109.7(9) . . ?
C4 F42 Cs1 119.4(6) . 2_556 ?
C2 F21 Cs1 120.3(5) . 2_556 ?
C2 F23 Cs1 109.5(6) . 1_565 ?
F22 C2 F21 107.9(11) . . ?
F22 C2 F23 106.2(9) . . ?
F21 C2 F23 101.6(11) . . ?
F22 C2 C1 111.8(10) . . ?
F21 C2 C1 115.6(9) . . ?
F23 C2 C1 112.8(10) . . ?
F41 C4 F42 106.8(12) . . ?
F41 C4 F43 108.4(12) . . ?
F42 C4 F43 104.5(13) . . ?
F41 C4 C3 112.1(12) . . ?
F42 C4 C3 113.5(10) . . ?
F43 C4 C3 111.0(11) . . ?
C11 N2 C31 117.1(11) . . ?
C11 N2 C41 114.6(11) . . ?
C31 N2 C41 110.3(10) . . ?
C11 N2 C21 94.8(11) . . ?
C31 N2 C21 112.2(10) . . ?
C41 N2 C21 106.5(10) . . ?
C12 C11 N2 110.2(13) . . ?
C12 C11 H11A 109.6 . . ?
N2 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
N2 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 110.2(13) . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
C13 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C14 C13 C12 117.1(15) . . ?
C14 C13 H13A 108.0 . . ?
C12 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
C12 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C22 C21 N2 124.2(17) . . ?
C22 C21 H21A 106.3 . . ?
N2 C21 H21A 106.3 . . ?
C22 C21 H21B 106.3 . . ?
N2 C21 H21B 106.3 . . ?
H21A C21 H21B 106.4 . . ?
C21 C22 C23 138.3(19) . . ?
C21 C22 H22A 102.5 . . ?
C23 C22 H22A 102.5 . . ?
C21 C22 H22B 102.5 . . ?
C23 C22 H22B 102.5 . . ?
H22A C22 H22B 104.9 . . ?
C24 C23 C22 93.3(15) . . ?
C24 C23 H23A 113.0 . . ?
C22 C23 H23A 113.0 . . ?
C24 C23 H23B 113.0 . . ?
C22 C23 H23B 113.0 . . ?
H23A C23 H23B 110.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 C31 N2 117.1(11) . . ?
C32 C31 H31A 108.0 . . ?
N2 C31 H31A 108.0 . . ?
C32 C31 H31B 108.0 . . ?
N2 C31 H31B 108.0 . . ?
H31A C31 H31B 107.3 . . ?
C31 C32 C33 113.1(12) . . ?
C31 C32 H32A 109.0 . . ?
C33 C32 H32A 109.0 . . ?
C31 C32 H32B 109.0 . . ?
C33 C32 H32B 109.0 . . ?
H32A C32 H32B 107.8 . . ?
C34 C33 C32 117.6(13) . . ?
C34 C33 H33A 107.9 . . ?
C32 C33 H33A 107.9 . . ?
C34 C33 H33B 107.9 . . ?
C32 C33 H33B 107.9 . . ?
H33A C33 H33B 107.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 C41 N2 123.9(13) . . ?
C42 C41 H41A 106.3 . . ?
N2 C41 H41A 106.3 . . ?
C42 C41 H41B 106.3 . . ?
N2 C41 H41B 106.3 . . ?
H41A C41 H41B 106.4 . . ?
C41 C42 C43 113.6(14) . . ?
C41 C42 H42A 108.8 . . ?
C43 C42 H42A 108.8 . . ?
C41 C42 H42B 108.8 . . ?
C43 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
C44 C43 C42 108.4(14) . . ?
C44 C43 H43A 110.0 . . ?
C42 C43 H43A 110.0 . . ?
C44 C43 H43B 110.0 . . ?
C42 C43 H43B 110.0 . . ?
H43A C43 H43B 108.4 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tc2 O5 C5 O8 -5.2(17) . . . . ?
Cs1 O5 C5 O8 -171.0(8) . . . . ?
Tc2 O5 C5 C6 175.6(7) . . . . ?
Cs1 O5 C5 C6 9.8(13) . . . . ?
O8 C5 C6 F61 -156.1(13) . . . . ?
O5 C5 C6 F61 23.2(18) . . . . ?
O8 C5 C6 F63 -29.8(18) . . . . ?
O5 C5 C6 F63 149.4(11) . . . . ?
O8 C5 C6 F62 78.2(16) . . . . ?
O5 C5 C6 F62 -102.5(13) . . . . ?
Cs1 F83 C8 F82 115.4(9) . . . . ?
Cs1 F83 C8 F81 -136.5(8) . . . . ?
Cs1 F83 C8 C7 -8.5(19) . . . . ?
Tc2 O4 C7 O9 -0.8(17) . . . . ?
Cs1 O4 C7 O9 175.8(8) . . . . ?
Tc2 O4 C7 C8 177.7(7) . . . . ?
Cs1 O4 C7 C8 -5.8(15) . . . . ?
F83 C8 C7 O9 -172.9(13) . . . . ?
F82 C8 C7 O9 66.1(16) . . . . ?
F81 C8 C7 O9 -45.1(16) . . . . ?
F83 C8 C7 O4 8.5(18) . . . . ?
F82 C8 C7 O4 -112.6(12) . . . . ?
F81 C8 C7 O4 136.3(11) . . . . ?
F63 C6 F61 Cs1 -170.2(8) . . . . ?
F62 C6 F61 Cs1 87.4(10) . . . . ?
C5 C6 F61 Cs1 -40.6(17) . . . . ?
Cs1 O6 C1 O2 101.8(10) 1_565 . . . ?
Cs1 O6 C1 C2 -75.6(9) 1_565 . . . ?
Tc2 O2 C1 O6 12.2(13) . . . . ?
Cs1 O2 C1 O6 -116.4(10) 2_556 . . . ?
Tc2 O2 C1 C2 -170.3(6) . . . . ?
Cs1 O2 C1 C2 61.1(9) 2_556 . . . ?
Tc2 O2 C1 Cs1 73.6(7) . . . 1_565 ?
Cs1 O2 C1 Cs1 -55.0(7) 2_556 . . 1_565 ?
Cs1 O7 C3 O3 -102.4(11) 1_565 . . . ?
Cs1 O7 C3 C4 78.7(11) 1_565 . . . ?
Tc2 O3 C3 O7 -7.9(15) . . . . ?
Cs1 O3 C3 O7 108.6(11) 2_556 . . . ?
Tc2 O3 C3 C4 171.1(8) . . . . ?
Cs1 O3 C3 C4 -72.4(9) 2_556 . . . ?
Cs1 F21 C2 F22 -132.3(7) 2_556 . . . ?
Cs1 F21 C2 F23 116.3(7) 2_556 . . . ?
Cs1 F21 C2 C1 -6.3(13) 2_556 . . . ?
Cs1 F23 C2 F22 143.2(8) 1_565 . . . ?
Cs1 F23 C2 F21 -104.0(7) 1_565 . . . ?
Cs1 F23 C2 C1 20.4(12) 1_565 . . . ?
O6 C1 C2 F22 -90.3(12) . . . . ?
O2 C1 C2 F22 91.9(11) . . . . ?
Cs1 C1 C2 F22 -138.3(9) 1_565 . . . ?
O6 C1 C2 F21 145.7(10) . . . . ?
O2 C1 C2 F21 -32.1(13) . . . . ?
Cs1 C1 C2 F21 97.7(9) 1_565 . . . ?
O6 C1 C2 F23 29.3(15) . . . . ?
O2 C1 C2 F23 -148.5(10) . . . . ?
Cs1 C1 C2 F23 -18.7(11) 1_565 . . . ?
Cs1 F42 C4 F41 127.0(8) 2_556 . . . ?
Cs1 F42 C4 F43 -118.3(8) 2_556 . . . ?
Cs1 F42 C4 C3 2.8(15) 2_556 . . . ?
O7 C3 C4 F41 99.9(13) . . . . ?
O3 C3 C4 F41 -79.2(13) . . . . ?
O7 C3 C4 F42 -138.9(11) . . . . ?
O3 C3 C4 F42 41.9(15) . . . . ?
O7 C3 C4 F43 -21.5(18) . . . . ?
O3 C3 C4 F43 159.4(12) . . . . ?
C31 N2 C11 C12 -71.3(17) . . . . ?
C41 N2 C11 C12 60.3(18) . . . . ?
C21 N2 C11 C12 170.8(14) . . . . ?
N2 C11 C12 C13 176.4(14) . . . . ?
C11 C12 C13 C14 173.1(18) . . . . ?
C11 N2 C21 C22 -179.0(16) . . . . ?
C31 N2 C21 C22 59.2(18) . . . . ?
C41 N2 C21 C22 -61.6(18) . . . . ?
N2 C21 C22 C23 154.9(17) . . . . ?
C21 C22 C23 C24 50(3) . . . . ?
C11 N2 C31 C32 -51.1(15) . . . . ?
C41 N2 C31 C32 175.5(11) . . . . ?
C21 N2 C31 C32 56.9(14) . . . . ?
N2 C31 C32 C33 173.5(11) . . . . ?
C31 C32 C33 C34 177.8(13) . . . . ?
C11 N2 C41 C42 -96.8(18) . . . . ?
C31 N2 C41 C42 37.9(18) . . . . ?
C21 N2 C41 C42 159.9(15) . . . . ?
N2 C41 C42 C43 -179.9(12) . . . . ?
C41 C42 C43 C44 177.3(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11B O9 0.97 2.38 3.33(2) 165.4 .
C21 H21A O9 0.97 2.67 3.577(19) 156.2 .

_refine_diff_density_max         0.533
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_tcnopypph2tfa
_audit_block_doi                 10.5517/ccdc.csd.cc1phw68
_database_code_depnum_ccdc_archive 'CCDC 1564390'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT03084C 2017
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT420_tcnopypph2tfa       
;
PROBLEM: D-H Without Acceptor      *O9     -- *H9     ...     Please Check 
RESPONSE: This results from the incomplete occupation of a solvent water molecule
;

#end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H28 F6 N3 O5 P2 Tc, C0.5 H2 O0.5, O0.25'
_chemical_formula_sum            'C38.50 H30 F6 N3 O5.75 P2 Tc'
_chemical_formula_weight         900.59

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.863(2)
_cell_length_b                   10.6900(10)
_cell_length_c                   29.057(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.96
_cell_angle_gamma                90
_cell_volume                     7628.7(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9967
_cell_measurement_theta_min      0.7138
_cell_measurement_theta_max      0.7450

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_F_000             3640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.541
_shelx_estimated_absorpt_T_min   0.774
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            116573
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.237
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9338
_reflns_number_gt                7402
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ortep'
_computing_publication_material  WingX
_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)+(0.0331P)²+54.5908P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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         9338
_refine_ls_number_parameters     515
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc1 Tc 0.41613(2) 0.62900(2) 0.39442(2) 0.01361(7) Uani 1 1 d . . . . .
P2 P 0.36721(3) 0.47164(7) 0.42872(3) 0.01559(17) Uani 1 1 d . . . . .
P1 P 0.35701(3) 0.80824(7) 0.39042(3) 0.01547(17) Uani 1 1 d . . . . .
O1 O 0.47038(10) 0.6799(2) 0.48917(8) 0.0233(5) Uani 1 1 d . . . . .
O4 O 0.37405(10) 0.5997(2) 0.32665(8) 0.0267(6) Uani 1 1 d . . . . .
O2 O 0.47562(9) 0.7100(2) 0.35787(8) 0.0205(5) Uani 1 1 d . . . . .
O3 O 0.50292(10) 0.8710(2) 0.40628(9) 0.0285(6) Uani 1 1 d . . . . .
N2 N 0.45352(11) 0.4440(2) 0.39393(9) 0.0171(6) Uani 1 1 d . . . . .
N1 N 0.44856(11) 0.6622(2) 0.45071(9) 0.0160(5) Uani 1 1 d . . . . .
N3 N 0.26480(12) 0.6864(3) 0.40090(11) 0.0263(7) Uani 1 1 d . . . . .
C40 C 0.42226(12) 0.3687(3) 0.41655(11) 0.0173(6) Uani 1 1 d . . . . .
C34 C 0.36926(13) 0.4806(3) 0.49128(11) 0.0177(6) Uani 1 1 d . . . . .
C17 C 0.35592(13) 0.8951(3) 0.44450(11) 0.0169(6) Uani 1 1 d . . . . .
C41 C 0.43282(14) 0.2428(3) 0.42262(12) 0.0228(7) Uani 1 1 d . . . . .
H41 H 0.4102 0.1913 0.4381 0.027 Uiso 1 1 calc R U . . .
C22 C 0.40585(14) 0.9331(3) 0.46933(11) 0.0197(7) Uani 1 1 d . . . . .
H22 H 0.4388 0.9102 0.4588 0.024 Uiso 1 1 calc R U . . .
C11 C 0.36603(13) 0.9312(3) 0.34856(11) 0.0180(6) Uani 1 1 d . . . . .
C39 C 0.39807(14) 0.3983(3) 0.52262(13) 0.0245(7) Uani 1 1 d . . . . .
H39 H 0.4174 0.3306 0.5117 0.029 Uiso 1 1 calc R U . . .
C23 C 0.28582(14) 0.7612(3) 0.37145(13) 0.0219(7) Uani 1 1 d . . . . .
C35 C 0.34141(14) 0.5807(3) 0.50785(13) 0.0250(7) Uani 1 1 d . . . . .
H35 H 0.3216 0.6377 0.4865 0.030 Uiso 1 1 calc R U . . .
C28 C 0.30496(13) 0.3877(3) 0.40706(12) 0.0203(7) Uani 1 1 d . . . . .
C29 C 0.27848(15) 0.4093(3) 0.36182(13) 0.0266(8) Uani 1 1 d . . . . .
H29 H 0.2921 0.4707 0.3430 0.032 Uiso 1 1 calc R U . . .
C12 C 0.34669(15) 1.0519(3) 0.35371(12) 0.0248(7) Uani 1 1 d . . . . .
H12 H 0.3284 1.0711 0.3792 0.030 Uiso 1 1 calc R U . . .
C36 C 0.34273(15) 0.5965(4) 0.55509(13) 0.0311(9) Uani 1 1 d . . . . .
H36 H 0.3242 0.6651 0.5663 0.037 Uiso 1 1 calc R U . . .
C1 C 0.50237(14) 0.8081(3) 0.37126(12) 0.0225(7) Uani 1 1 d . . . . .
C44 C 0.49583(14) 0.3961(3) 0.37673(12) 0.0228(7) Uani 1 1 d . . . . .
H44 H 0.5171 0.4489 0.3604 0.027 Uiso 1 1 calc R U . . .
C32 C 0.23801(15) 0.2304(4) 0.41677(14) 0.0297(8) Uani 1 1 d . . . . .
H32 H 0.2240 0.1693 0.4355 0.036 Uiso 1 1 calc R U . . .
C43 C 0.50917(14) 0.2701(3) 0.38245(13) 0.0268(8) Uani 1 1 d . . . . .
H43 H 0.5398 0.2374 0.3706 0.032 Uiso 1 1 calc R U . . .
C33 C 0.28451(14) 0.2979(3) 0.43473(13) 0.0257(8) Uani 1 1 d . . . . .
H33 H 0.3022 0.2830 0.4656 0.031 Uiso 1 1 calc R U . . .
C42 C 0.47758(15) 0.1927(3) 0.40547(13) 0.0279(8) Uani 1 1 d . . . . .
H42 H 0.4862 0.1064 0.4096 0.034 Uiso 1 1 calc R U . . .
C13 C 0.35406(17) 1.1442(3) 0.32177(13) 0.0306(8) Uani 1 1 d . . . . .
H13 H 0.3408 1.2263 0.3255 0.037 Uiso 1 1 calc R U . . .
C16 C 0.39150(16) 0.9048(3) 0.31027(12) 0.0274(8) Uani 1 1 d . . . . .
H16 H 0.4040 0.8223 0.3058 0.033 Uiso 1 1 calc R U . . .
C30 C 0.23224(16) 0.3412(4) 0.34420(14) 0.0328(9) Uani 1 1 d . . . . .
H30 H 0.2144 0.3557 0.3133 0.039 Uiso 1 1 calc R U . . .
C21 C 0.40729(16) 1.0049(3) 0.50956(12) 0.0245(7) Uani 1 1 d . . . . .
H21 H 0.4413 1.0310 0.5264 0.029 Uiso 1 1 calc R U . . .
C18 C 0.30807(14) 0.9282(3) 0.46038(13) 0.0250(7) Uani 1 1 d . . . . .
H18 H 0.2740 0.9016 0.4439 0.030 Uiso 1 1 calc R U . . .
C31 C 0.21219(15) 0.2522(4) 0.37171(15) 0.0329(9) Uani 1 1 d . . . . .
H31 H 0.1805 0.2058 0.3596 0.040 Uiso 1 1 calc R U . . .
C38 C 0.39877(16) 0.4146(4) 0.57020(13) 0.0314(9) Uani 1 1 d . . . . .
H38 H 0.4185 0.3578 0.5916 0.038 Uiso 1 1 calc R U . . .
C37 C 0.37104(15) 0.5126(4) 0.58649(13) 0.0297(8) Uani 1 1 d . . . . .
H37 H 0.3713 0.5228 0.6190 0.036 Uiso 1 1 calc R U . . .
C14 C 0.38062(17) 1.1176(4) 0.28449(13) 0.0315(8) Uani 1 1 d . . . . .
H14 H 0.3863 1.1816 0.2631 0.038 Uiso 1 1 calc R U . . .
C20 C 0.35932(17) 1.0382(4) 0.52505(13) 0.0303(8) Uani 1 1 d . . . . .
H20 H 0.3603 1.0869 0.5525 0.036 Uiso 1 1 calc R U . . .
C19 C 0.30992(17) 1.0002(4) 0.50035(14) 0.0322(9) Uani 1 1 d . . . . .
H19 H 0.2770 1.0235 0.5108 0.039 Uiso 1 1 calc R U . . .
C27 C 0.21378(15) 0.6451(4) 0.38748(16) 0.0341(9) Uani 1 1 d . . . . .
H27 H 0.1981 0.5924 0.4082 0.041 Uiso 1 1 calc R U . . .
C3 C 0.37835(18) 0.5297(4) 0.29282(13) 0.0330(9) Uani 1 1 d . . . . .
C24 C 0.25723(18) 0.7965(4) 0.32852(16) 0.0442(12) Uani 1 1 d . . . . .
H24 H 0.2733 0.8500 0.3084 0.053 Uiso 1 1 calc R U . . .
C15 C 0.39878(18) 0.9979(4) 0.27859(13) 0.0349(9) Uani 1 1 d . . . . .
H15 H 0.4164 0.9790 0.2527 0.042 Uiso 1 1 calc R U . . .
C26 C 0.18272(17) 0.6749(4) 0.34521(18) 0.0447(12) Uani 1 1 d . . . . .
H26 H 0.1469 0.6427 0.3369 0.054 Uiso 1 1 calc R U . . .
C2 C 0.53996(16) 0.8510(4) 0.33718(14) 0.0346(9) Uani 1 1 d D . . . .
C25 C 0.2049(2) 0.7519(5) 0.3157(2) 0.0626(17) Uani 1 1 d . . . . .
H25 H 0.1844 0.7747 0.2865 0.075 Uiso 1 1 calc R U . . .
F1 F 0.5231(2) 0.8179(6) 0.29348(19) 0.0664(8) Uani 0.593(3) 1 d D . P A 1
F2 F 0.5899(2) 0.8291(6) 0.3512(2) 0.0664(8) Uani 0.593(3) 1 d D . P A 1
F3 F 0.5369(2) 0.9801(5) 0.33285(19) 0.0664(8) Uani 0.593(3) 1 d D . P A 1
F1A F 0.5172(3) 0.8983(8) 0.2990(3) 0.0664(8) Uani 0.407(3) 1 d D . P A 2
F2A F 0.5688(3) 0.7462(7) 0.3226(3) 0.0664(8) Uani 0.407(3) 1 d D . P A 2
F3A F 0.5841(3) 0.9128(8) 0.3573(3) 0.0664(8) Uani 0.407(3) 1 d D . P A 2
C4 C 0.3430(2) 0.5672(4) 0.24803(16) 0.0544(14) Uani 1 1 d D . . . .
F5 F 0.2935(3) 0.4964(8) 0.2550(2) 0.0653(8) Uani 0.438(7) 1 d D . P B 1
F6 F 0.3231(4) 0.6858(7) 0.2448(2) 0.0653(8) Uani 0.438(7) 1 d D . P B 1
F7 F 0.3655(4) 0.5122(9) 0.2133(3) 0.0653(8) Uani 0.438(7) 1 d D . P B 1
O5 O 0.4202(5) 0.4724(12) 0.2876(3) 0.064(3) Uani 0.438(7) 1 d . . P B 1
F5A F 0.3511(3) 0.5228(7) 0.2073(2) 0.0653(8) Uani 0.562(7) 1 d D . P B 2
F6A F 0.2919(3) 0.5510(7) 0.24400(19) 0.0653(8) Uani 0.562(7) 1 d D . P B 2
F7A F 0.3524(3) 0.6915(5) 0.23866(19) 0.0653(8) Uani 0.562(7) 1 d D . P B 2
O5A O 0.3917(3) 0.4177(6) 0.2940(2) 0.0471(19) Uani 0.562(7) 1 d . . P B 2
O9 O 0.4404(3) 0.3112(6) 0.2126(2) 0.0445(15) Uiso 0.5 1 d . . P C -1
H9 H 0.4428 0.3893 0.2155 0.067 Uiso 0.5 1 calc R U P C -1
C9 C 0.4862(4) 0.2584(10) 0.2335(3) 0.050(2) Uiso 0.5 1 d . . P C -1
H9A H 0.5137 0.3233 0.2425 0.075 Uiso 0.5 1 calc R U P C -1
H9B H 0.4996 0.1996 0.2120 0.075 Uiso 0.5 1 calc R U P C -1
H9C H 0.4791 0.2135 0.2613 0.075 Uiso 0.5 1 calc R U P C -1
O10 O 0.4828(8) 0.5390(19) 0.2339(7) 0.097(6) Uiso 0.25 1 d . . P . .


_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
Tc1 N1 1.744(3) . ?
Tc1 O4 2.105(2) . ?
Tc1 O2 2.134(2) . ?
Tc1 N2 2.187(3) . ?
Tc1 P2 2.3833(9) . ?
Tc1 P1 2.4068(8) . ?
P2 C34 1.813(3) . ?
P2 C28 1.815(3) . ?
P2 C40 1.833(3) . ?
P1 C11 1.829(3) . ?
P1 C17 1.829(3) . ?
P1 C23 1.840(3) . ?
O1 N1 1.179(3) . ?
O4 C3 1.254(4) . ?
O2 C1 1.270(4) . ?
O3 C1 1.218(4) . ?
N2 C44 1.335(4) . ?
N2 C40 1.357(4) . ?
N3 C23 1.336(5) . ?
N3 C27 1.342(5) . ?
C40 C41 1.377(5) . ?
C34 C39 1.384(5) . ?
C34 C35 1.400(5) . ?
C17 C18 1.388(5) . ?
C17 C22 1.396(5) . ?
C41 C42 1.395(5) . ?
C41 H41 0.9500 . ?
C22 C21 1.394(5) . ?
C22 H22 0.9500 . ?
C11 C16 1.392(5) . ?
C11 C12 1.393(5) . ?
C39 C38 1.391(5) . ?
C39 H39 0.9500 . ?
C23 C24 1.388(5) . ?
C35 C36 1.378(5) . ?
C35 H35 0.9500 . ?
C28 C29 1.395(5) . ?
C28 C33 1.398(5) . ?
C29 C30 1.389(5) . ?
C29 H29 0.9500 . ?
C12 C13 1.386(5) . ?
C12 H12 0.9500 . ?
C36 C37 1.390(6) . ?
C36 H36 0.9500 . ?
C1 C2 1.534(5) . ?
C44 C43 1.391(5) . ?
C44 H44 0.9500 . ?
C32 C31 1.385(6) . ?
C32 C33 1.394(5) . ?
C32 H32 0.9500 . ?
C43 C42 1.383(5) . ?
C43 H43 0.9500 . ?
C33 H33 0.9500 . ?
C42 H42 0.9500 . ?
C13 C14 1.383(5) . ?
C13 H13 0.9500 . ?
C16 C15 1.387(5) . ?
C16 H16 0.9500 . ?
C30 C31 1.385(6) . ?
C30 H30 0.9500 . ?
C21 C20 1.385(5) . ?
C21 H21 0.9500 . ?
C18 C19 1.388(5) . ?
C18 H18 0.9500 . ?
C31 H31 0.9500 . ?
C38 C37 1.378(6) . ?
C38 H38 0.9500 . ?
C37 H37 0.9500 . ?
C14 C15 1.377(5) . ?
C14 H14 0.9500 . ?
C20 C19 1.384(6) . ?
C20 H20 0.9500 . ?
C19 H19 0.9500 . ?
C27 C26 1.382(6) . ?
C27 H27 0.9500 . ?
C3 O5 1.236(9) . ?
C3 O5A 1.241(7) . ?
C3 C4 1.507(6) . ?
C24 C25 1.382(6) . ?
C24 H24 0.9500 . ?
C15 H15 0.9500 . ?
C26 C25 1.364(7) . ?
C26 H26 0.9500 . ?
C2 F2 1.266(6) . ?
C2 F1A 1.268(8) . ?
C2 F1 1.322(6) . ?
C2 F3A 1.335(8) . ?
C2 F3 1.386(6) . ?
C2 F2A 1.430(8) . ?
C25 H25 0.9500 . ?
C4 F6A 1.269(7) . ?
C4 F5A 1.320(8) . ?
C4 F6 1.359(8) . ?
C4 F7 1.362(9) . ?
C4 F7A 1.383(7) . ?
C4 F5 1.486(9) . ?
O9 C9 1.330(11) . ?
O9 H9 0.8400 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O10 O10 1.17(4) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Tc1 O4 176.25(11) . . ?
N1 Tc1 O2 97.42(11) . . ?
O4 Tc1 O2 82.92(10) . . ?
N1 Tc1 N2 93.18(11) . . ?
O4 Tc1 N2 90.54(9) . . ?
O2 Tc1 N2 92.04(9) . . ?
N1 Tc1 P2 86.74(9) . . ?
O4 Tc1 P2 94.28(8) . . ?
O2 Tc1 P2 158.89(7) . . ?
N2 Tc1 P2 67.00(7) . . ?
N1 Tc1 P1 94.18(9) . . ?
O4 Tc1 P1 82.08(7) . . ?
O2 Tc1 P1 96.80(7) . . ?
N2 Tc1 P1 167.67(7) . . ?
P2 Tc1 P1 103.56(3) . . ?
C34 P2 C28 105.25(15) . . ?
C34 P2 C40 108.65(15) . . ?
C28 P2 C40 104.96(15) . . ?
C34 P2 Tc1 116.46(11) . . ?
C28 P2 Tc1 131.86(12) . . ?
C40 P2 Tc1 84.16(11) . . ?
C11 P1 C17 103.07(14) . . ?
C11 P1 C23 102.08(16) . . ?
C17 P1 C23 104.71(16) . . ?
C11 P1 Tc1 117.86(11) . . ?
C17 P1 Tc1 116.95(10) . . ?
C23 P1 Tc1 110.40(11) . . ?
C3 O4 Tc1 137.0(3) . . ?
C1 O2 Tc1 123.6(2) . . ?
C44 N2 C40 119.9(3) . . ?
C44 N2 Tc1 135.2(2) . . ?
C40 N2 Tc1 104.9(2) . . ?
O1 N1 Tc1 177.4(2) . . ?
C23 N3 C27 117.2(3) . . ?
N2 C40 C41 121.9(3) . . ?
N2 C40 P2 103.8(2) . . ?
C41 C40 P2 134.0(3) . . ?
C39 C34 C35 119.5(3) . . ?
C39 C34 P2 123.9(3) . . ?
C35 C34 P2 116.6(3) . . ?
C18 C17 C22 119.6(3) . . ?
C18 C17 P1 122.9(3) . . ?
C22 C17 P1 117.5(2) . . ?
C40 C41 C42 118.5(3) . . ?
C40 C41 H41 120.8 . . ?
C42 C41 H41 120.8 . . ?
C21 C22 C17 119.9(3) . . ?
C21 C22 H22 120.1 . . ?
C17 C22 H22 120.1 . . ?
C16 C11 C12 118.8(3) . . ?
C16 C11 P1 120.2(2) . . ?
C12 C11 P1 121.0(3) . . ?
C34 C39 C38 120.0(3) . . ?
C34 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
N3 C23 C24 122.8(3) . . ?
N3 C23 P1 115.2(3) . . ?
C24 C23 P1 121.9(3) . . ?
C36 C35 C34 120.0(3) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C29 C28 C33 119.7(3) . . ?
C29 C28 P2 119.8(3) . . ?
C33 C28 P2 120.5(3) . . ?
C30 C29 C28 120.2(4) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C13 C12 C11 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C35 C36 C37 120.4(4) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
O3 C1 O2 130.4(3) . . ?
O3 C1 C2 116.5(3) . . ?
O2 C1 C2 113.1(3) . . ?
N2 C44 C43 120.9(3) . . ?
N2 C44 H44 119.6 . . ?
C43 C44 H44 119.6 . . ?
C31 C32 C33 120.2(4) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C42 C43 C44 119.6(3) . . ?
C42 C43 H43 120.2 . . ?
C44 C43 H43 120.2 . . ?
C32 C33 C28 119.7(4) . . ?
C32 C33 H33 120.2 . . ?
C28 C33 H33 120.2 . . ?
C43 C42 C41 119.2(3) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C16 C11 120.5(3) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C31 C30 C29 119.9(4) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C20 C21 C22 120.2(3) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C17 C18 C19 120.1(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C30 C31 C32 120.4(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C37 C38 C39 120.5(4) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 H38 119.7 . . ?
C38 C37 C36 119.6(3) . . ?
C38 C37 H37 120.2 . . ?
C36 C37 H37 120.2 . . ?
C15 C14 C13 119.6(4) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C19 C20 C21 119.7(3) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C20 C19 C18 120.5(4) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
N3 C27 C26 123.6(4) . . ?
N3 C27 H27 118.2 . . ?
C26 C27 H27 118.2 . . ?
O5 C3 O4 124.7(6) . . ?
O5A C3 O4 127.5(5) . . ?
O5 C3 C4 114.5(5) . . ?
O5A C3 C4 113.5(4) . . ?
O4 C3 C4 114.1(4) . . ?
C25 C24 C23 118.5(4) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C14 C15 C16 120.4(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C25 C26 C27 118.2(4) . . ?
C25 C26 H26 120.9 . . ?
C27 C26 H26 120.9 . . ?
F2 C2 F1 114.0(5) . . ?
F1A C2 F3A 114.2(5) . . ?
F2 C2 F3 104.6(4) . . ?
F1 C2 F3 100.0(4) . . ?
F1A C2 F2A 103.3(6) . . ?
F3A C2 F2A 95.8(5) . . ?
F2 C2 C1 113.7(4) . . ?
F1A C2 C1 116.7(5) . . ?
F1 C2 C1 114.0(4) . . ?
F3A C2 C1 114.0(4) . . ?
F3 C2 C1 109.0(4) . . ?
F2A C2 C1 110.0(4) . . ?
C26 C25 C24 119.6(4) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
F6A C4 F5A 99.1(5) . . ?
F6 C4 F7 122.6(6) . . ?
F6A C4 F7A 108.1(5) . . ?
F5A C4 F7A 96.6(5) . . ?
F6 C4 F5 100.6(6) . . ?
F7 C4 F5 109.0(6) . . ?
F6A C4 C3 119.0(5) . . ?
F5A C4 C3 121.9(5) . . ?
F6 C4 C3 117.7(4) . . ?
F7 C4 C3 105.9(5) . . ?
F7A C4 C3 109.4(4) . . ?
F5 C4 C3 97.5(4) . . ?
C9 O9 H9 109.5 . . ?
O9 C9 H9A 109.5 . . ?
O9 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O9 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9 O10 0.84 1.92 2.69(2) 152.0 .
C9 H9A O10 0.98 2.43 3.00(2) 116.6 .
C9 H9A O10 0.98 2.40 3.20(2) 138.4 2_655

_refine_diff_density_max         1.484
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.105

####################################################################### 
# 
# 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_tcnodppetfa
_audit_block_doi                 10.5517/ccdc.csd.cc1phw57
_database_code_depnum_ccdc_archive 'CCDC 1564389'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT03084C 2017
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT910_tcnodppetfa         
;
PROBLEM: _Missing # of FCF Reflection(s) Below Theta(Min) 17 Note
RESPONSE: This is a problem of the automatic datacollection routine of the STOE IPDS2T system
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H48 F3 N O3 P4 Tc, P F6'
_chemical_formula_sum            'C54 H48 F9 N O3 P5 Tc'
_chemical_formula_weight         1182.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7590 '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/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   19.479(2)
_cell_length_b                   12.1460(10)
_cell_length_c                   25.141(2)
_cell_angle_alpha                90
_cell_angle_beta                 118.670(10)
_cell_angle_gamma                90
_cell_volume                     5218.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    15339
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.28

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             2408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.506
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            39491
_diffrn_reflns_av_unetI/netI     0.1634
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.136
_diffrn_reflns_theta_max         32.769
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.727
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.727
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.727
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             14050
_reflns_number_gt                5689
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ortep
_computing_publication_material  WingX
_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)+(0.1242P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_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       0.0032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14050
_refine_ls_number_parameters     561
_refine_ls_number_restraints     311
_refine_ls_R_factor_all          0.1943
_refine_ls_R_factor_gt           0.0847
_refine_ls_wR_factor_ref         0.2483
_refine_ls_wR_factor_gt          0.2062
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_restrained_S_all      0.914
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6434(4) 0.0849(6) 0.4018(3) 0.051(2) Uani 1 1 d D . . . .
H1A H 0.6104 0.0915 0.4208 0.062 Uiso 1 1 calc R U . . .
H1B H 0.6098 0.0723 0.3588 0.062 Uiso 1 1 calc R U . . .
C2 C 0.6971(4) -0.0117(6) 0.4285(3) 0.055(2) Uani 1 1 d D . . . .
H2A H 0.7362 -0.0142 0.4151 0.066 Uiso 1 1 calc R U . . .
H2B H 0.6682 -0.0804 0.4181 0.066 Uiso 1 1 calc R U . . .
C3 C 0.8662(4) 0.3569(7) 0.6507(3) 0.054(2) Uani 1 1 d . . . . .
H3A H 0.8177 0.3785 0.6498 0.064 Uiso 1 1 calc R U . . .
H3B H 0.9088 0.3674 0.6915 0.064 Uiso 1 1 calc R U . . .
C4 C 0.8803(4) 0.4282(7) 0.6038(3) 0.054(2) Uani 1 1 d . . . . .
H4A H 0.9294 0.4064 0.6057 0.064 Uiso 1 1 calc R U . . .
H4B H 0.8842 0.5054 0.6148 0.064 Uiso 1 1 calc R U . . .
C5 C 0.6384(4) 0.2438(7) 0.5476(4) 0.058(2) Uani 1 1 d D . . . .
C6 C 0.6023(5) 0.2762(10) 0.5922(5) 0.081(3) Uani 1 1 d D . . . .
C11 C 0.6328(2) 0.3160(4) 0.3752(2) 0.048(2) Uani 1 1 d G . . . .
C12 C 0.6562(2) 0.4104(4) 0.3569(2) 0.061(2) Uani 1 1 d G . . . .
H12 H 0.7059 0.4142 0.3605 0.073 Uiso 1 1 calc R U . . .
C13 C 0.6051(3) 0.4989(4) 0.3332(3) 0.079(3) Uani 1 1 d G . . . .
H13 H 0.6207 0.5621 0.3210 0.095 Uiso 1 1 calc R U . . .
C14 C 0.5308(3) 0.4932(4) 0.3278(3) 0.080(3) Uani 1 1 d G . . . .
H14 H 0.4967 0.5524 0.3119 0.096 Uiso 1 1 calc R U . . .
C15 C 0.5075(2) 0.3988(5) 0.3461(3) 0.083(3) Uani 1 1 d G . . . .
H15 H 0.4577 0.3950 0.3425 0.100 Uiso 1 1 calc R U . . .
C16 C 0.5585(2) 0.3102(4) 0.3698(3) 0.066(3) Uani 1 1 d G . . . .
H16 H 0.5429 0.2471 0.3821 0.080 Uiso 1 1 calc R U . . .
C21 C 0.7471(3) 0.1967(5) 0.3525(2) 0.055(2) Uani 1 1 d G . . . .
C22 C 0.8026(3) 0.2748(4) 0.3588(2) 0.061(2) Uani 1 1 d G . . . .
H22 H 0.8188 0.3275 0.3893 0.073 Uiso 1 1 calc R U . . .
C23 C 0.8341(3) 0.2743(5) 0.3195(3) 0.084(3) Uani 1 1 d G . . . .
H23 H 0.8713 0.3265 0.3237 0.101 Uiso 1 1 calc R U . . .
C24 C 0.8099(4) 0.1956(6) 0.2739(3) 0.103(4) Uani 1 1 d G . . . .
H24 H 0.8310 0.1952 0.2476 0.124 Uiso 1 1 calc R U . . .
C25 C 0.7544(4) 0.1175(5) 0.2676(2) 0.075(3) Uani 1 1 d G . . . .
H25 H 0.7382 0.0649 0.2370 0.090 Uiso 1 1 calc R U . . .
C26 C 0.7229(3) 0.1181(4) 0.3069(2) 0.059(2) Uani 1 1 d G . . . .
H26 H 0.6857 0.0658 0.3027 0.071 Uiso 1 1 calc R U . . .
C31 C 0.8125(2) -0.0830(4) 0.5280(2) 0.054(2) Uani 1 1 d G U . . .
C32 C 0.8318(3) -0.1423(5) 0.5806(2) 0.074(2) Uani 1 1 d G U . . .
H32 H 0.8032 -0.1325 0.6011 0.089 Uiso 1 1 calc R U . . .
C33 C 0.8939(3) -0.2162(5) 0.6027(3) 0.096(3) Uani 1 1 d G U . . .
H33 H 0.9068 -0.2559 0.6378 0.115 Uiso 1 1 calc R U . . .
C34 C 0.9366(3) -0.2308(5) 0.5721(3) 0.101(4) Uani 1 1 d G U . . .
H34 H 0.9782 -0.2802 0.5868 0.121 Uiso 1 1 calc R U . . .
C35 C 0.9173(3) -0.1715(5) 0.5195(3) 0.089(3) Uani 1 1 d G U . . .
H35 H 0.9460 -0.1812 0.4990 0.107 Uiso 1 1 calc R U . . .
C36 C 0.8553(3) -0.0976(5) 0.4975(2) 0.068(2) Uani 1 1 d G U . . .
H36 H 0.8424 -0.0579 0.4623 0.082 Uiso 1 1 calc R U . . .
C41 C 0.6749(2) -0.0209(5) 0.5517(3) 0.061(2) Uani 1 1 d G U . . .
C42 C 0.6057(3) -0.0751(5) 0.5134(2) 0.076(3) Uani 1 1 d G U . . .
H42 H 0.5943 -0.0921 0.4740 0.091 Uiso 1 1 calc R U . . .
C43 C 0.5536(2) -0.1040(5) 0.5342(3) 0.088(3) Uani 1 1 d G U . . .
H43 H 0.5073 -0.1403 0.5085 0.106 Uiso 1 1 calc R U . . .
C44 C 0.5707(3) -0.0787(5) 0.5932(3) 0.093(3) Uani 1 1 d G U . . .
H44 H 0.5358 -0.0980 0.6070 0.112 Uiso 1 1 calc R U . . .
C45 C 0.6399(4) -0.0245(6) 0.6315(3) 0.094(3) Uani 1 1 d G U . . .
H45 H 0.6513 -0.0076 0.6709 0.113 Uiso 1 1 calc R U . . .
C46 C 0.6920(3) 0.0044(5) 0.6107(3) 0.077(3) Uani 1 1 d G U . . .
H46 H 0.7383 0.0406 0.6364 0.093 Uiso 1 1 calc R U . . .
C51 C 0.8360(3) 0.1407(5) 0.6908(2) 0.061(2) Uani 1 1 d G U . . .
C52 C 0.7885(3) 0.1862(5) 0.7122(3) 0.073(2) Uani 1 1 d G U . . .
H52 H 0.7682 0.2567 0.7003 0.087 Uiso 1 1 calc R U . . .
C53 C 0.7711(4) 0.1264(7) 0.7514(3) 0.098(3) Uani 1 1 d G U . . .
H53 H 0.7393 0.1568 0.7657 0.118 Uiso 1 1 calc R U . . .
C54 C 0.8014(4) 0.0210(6) 0.7692(3) 0.103(3) Uani 1 1 d G U . . .
H54 H 0.7898 -0.0190 0.7954 0.124 Uiso 1 1 calc R U . . .
C55 C 0.8490(4) -0.0245(4) 0.7478(3) 0.084(3) Uani 1 1 d G U . . .
H55 H 0.8692 -0.0950 0.7597 0.101 Uiso 1 1 calc R U . . .
C56 C 0.8663(3) 0.0353(5) 0.7086(3) 0.068(2) Uani 1 1 d G U . . .
H56 H 0.8981 0.0048 0.6943 0.081 Uiso 1 1 calc R U . . .
C61 C 0.9514(2) 0.1669(5) 0.6386(2) 0.056(2) Uani 1 1 d G U . . .
C62 C 1.0147(3) 0.2203(4) 0.6854(2) 0.067(2) Uani 1 1 d G U . . .
H62 H 1.0062 0.2785 0.7056 0.080 Uiso 1 1 calc R U . . .
C63 C 1.0905(2) 0.1866(5) 0.7021(2) 0.077(3) Uani 1 1 d G U . . .
H63 H 1.1328 0.2223 0.7334 0.093 Uiso 1 1 calc R U . . .
C64 C 1.1032(2) 0.0997(5) 0.6719(3) 0.076(3) Uani 1 1 d G U . . .
H64 H 1.1539 0.0772 0.6830 0.092 Uiso 1 1 calc R U . . .
C65 C 1.0399(3) 0.0463(5) 0.6250(3) 0.078(3) Uani 1 1 d G U . . .
H65 H 1.0484 -0.0119 0.6048 0.093 Uiso 1 1 calc R U . . .
C66 C 0.9641(2) 0.0800(4) 0.6084(2) 0.064(2) Uani 1 1 d G U . . .
H66 H 0.9218 0.0443 0.5770 0.077 Uiso 1 1 calc R U . . .
C71 C 0.8447(3) 0.4837(4) 0.4755(2) 0.057(2) Uani 1 1 d G U . . .
C72 C 0.8051(3) 0.5767(4) 0.4431(2) 0.065(2) Uani 1 1 d G U . . .
H72 H 0.7640 0.6054 0.4477 0.077 Uiso 1 1 calc R U . . .
C73 C 0.8268(4) 0.6267(4) 0.4037(2) 0.080(3) Uani 1 1 d G U . . .
H73 H 0.8003 0.6890 0.3820 0.096 Uiso 1 1 calc R U . . .
C74 C 0.8882(4) 0.5838(6) 0.3967(2) 0.090(3) Uani 1 1 d G U . . .
H74 H 0.9027 0.6173 0.3703 0.108 Uiso 1 1 calc R U . . .
C75 C 0.9278(3) 0.4908(5) 0.4291(3) 0.077(2) Uani 1 1 d G U . . .
H75 H 0.9688 0.4621 0.4244 0.093 Uiso 1 1 calc R U . . .
C76 C 0.9061(3) 0.4407(4) 0.4685(3) 0.062(2) Uani 1 1 d G U . . .
H76 H 0.9326 0.3785 0.4902 0.074 Uiso 1 1 calc R U . . .
C81 C 0.7362(3) 0.5018(5) 0.5422(3) 0.0540(19) Uani 1 1 d G U . . .
C82 C 0.7524(3) 0.5894(5) 0.5820(3) 0.075(3) Uani 1 1 d G U . . .
H82 H 0.8039 0.6065 0.6097 0.090 Uiso 1 1 calc R U . . .
C83 C 0.6915(4) 0.6514(5) 0.5806(3) 0.091(3) Uani 1 1 d G U . . .
H83 H 0.7023 0.7100 0.6072 0.109 Uiso 1 1 calc R U . . .
C84 C 0.6145(3) 0.6258(5) 0.5393(3) 0.087(3) Uani 1 1 d G U . . .
H84 H 0.5738 0.6673 0.5383 0.104 Uiso 1 1 calc R U . . .
C85 C 0.5983(2) 0.5383(5) 0.4994(3) 0.078(3) Uani 1 1 d G U . . .
H85 H 0.5467 0.5211 0.4717 0.093 Uiso 1 1 calc R U . . .
C86 C 0.6591(3) 0.4762(4) 0.5009(2) 0.065(2) Uani 1 1 d G U . . .
H86 H 0.6483 0.4176 0.4742 0.078 Uiso 1 1 calc R U . . .
F1 F 0.5101(5) -0.2266(5) 0.2552(4) 0.142(4) Uani 1 1 d . . . . .
F2 F 0.5138(4) -0.1044(6) 0.3277(3) 0.103(2) Uani 1 1 d . . . . .
F3 F 0.5948(3) -0.0971(6) 0.2807(2) 0.094(2) Uani 1 1 d . . . . .
F4 F 0.5097(4) 0.0306(5) 0.2647(3) 0.122(3) Uani 1 1 d . . . . .
F5 F 0.5064(3) -0.0913(7) 0.1913(2) 0.107(2) Uani 1 1 d . . . . .
F6 F 0.4241(3) -0.0976(7) 0.2364(3) 0.113(2) Uani 1 1 d . . . . .
N1 N 0.8529(3) 0.1836(5) 0.4936(3) 0.0491(16) Uani 1 1 d . U . . .
O1 O 0.9004(3) 0.1644(5) 0.4755(3) 0.0647(17) Uani 1 1 d . U . . .
O2 O 0.7052(3) 0.2470(5) 0.5656(3) 0.0579(15) Uani 1 1 d . U . . .
O3 O 0.5983(3) 0.2229(5) 0.4970(3) 0.0707(18) Uani 1 1 d . U . . .
P1 P 0.69615(9) 0.21099(18) 0.41198(8) 0.0454(5) Uani 1 1 d . . . . .
P2 P 0.74153(9) 0.01567(16) 0.50960(9) 0.0468(5) Uani 1 1 d . U . . .
P3 P 0.86128(9) 0.21238(19) 0.62752(8) 0.0478(5) Uani 1 1 d . . . . .
P4 P 0.80664(10) 0.41139(17) 0.53206(8) 0.0444(5) Uani 1 1 d . . . . .
P5 P 0.50932(11) -0.0992(2) 0.25979(10) 0.0579(6) Uani 1 1 d . . . . .
Tc1 Tc 0.78057(3) 0.21125(5) 0.51965(2) 0.03787(19) Uani 1 1 d . . . . .
F7 F 0.5348(6) 0.2348(12) 0.5831(6) 0.108(2) Uani 0.559(8) 1 d D . P A 1
F8 F 0.6376(7) 0.2501(13) 0.6542(6) 0.108(2) Uani 0.559(8) 1 d D . P A 1
F9 F 0.5905(7) 0.3804(12) 0.5996(6) 0.108(2) Uani 0.559(8) 1 d D . P A 1
F7A F 0.5353(8) 0.3163(16) 0.5677(7) 0.108(2) Uani 0.441(8) 1 d D . P A 2
F8A F 0.6109(9) 0.2133(15) 0.6364(8) 0.108(2) Uani 0.441(8) 1 d D . P A 2
F9A F 0.6427(9) 0.3712(14) 0.6256(7) 0.108(2) Uani 0.441(8) 1 d D . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.499(9) . ?
C1 P1 1.793(7) . ?
C2 P2 1.822(8) . ?
C3 C4 1.590(12) . ?
C3 P3 1.838(9) . ?
C4 P4 1.694(7) . ?
C5 O3 1.158(9) . ?
C5 O2 1.155(8) . ?
C5 C6 1.630(13) . ?
C6 F7A 1.245(17) . ?
C6 F8A 1.29(2) . ?
C6 F7 1.322(15) . ?
C6 F9 1.315(16) . ?
C6 F8 1.405(17) . ?
C6 F9A 1.421(19) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C11 P1 1.705(4) . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C21 P1 2.162(5) . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C31 P2 1.716(4) . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C41 P2 2.079(5) . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C51 C52 1.3900 . ?
C51 C56 1.3900 . ?
C51 P3 2.069(5) . ?
C52 C53 1.3900 . ?
C53 C54 1.3900 . ?
C54 C55 1.3900 . ?
C55 C56 1.3900 . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C61 P3 1.731(4) . ?
C62 C63 1.3900 . ?
C63 C64 1.3900 . ?
C64 C65 1.3900 . ?
C65 C66 1.3900 . ?
C71 C72 1.3900 . ?
C71 C76 1.3900 . ?
C71 P4 2.087(5) . ?
C72 C73 1.3900 . ?
C73 C74 1.3900 . ?
C74 C75 1.3900 . ?
C75 C76 1.3900 . ?
C81 C82 1.3900 . ?
C81 C86 1.3900 . ?
C81 P4 1.868(5) . ?
C82 C83 1.3900 . ?
C83 C84 1.3900 . ?
C84 C85 1.3900 . ?
C85 C86 1.3900 . ?
F1 P5 1.552(7) . ?
F2 P5 1.668(7) . ?
F3 P5 1.486(5) . ?
F4 P5 1.581(6) . ?
F5 P5 1.698(6) . ?
F6 P5 1.472(5) . ?
N1 O1 1.233(9) . ?
N1 Tc1 1.847(8) . ?
O2 Tc1 2.303(6) . ?
P1 Tc1 2.4002(18) . ?
P2 Tc1 2.470(2) . ?
P3 Tc1 2.3949(19) . ?
P4 Tc1 2.472(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
C2 C1 P1 112.1(5) . . ?
C1 C2 P2 102.3(5) . . ?
C4 C3 P3 106.6(5) . . ?
C3 C4 P4 111.4(5) . . ?
O3 C5 O2 118.4(9) . . ?
O3 C5 C6 121.5(7) . . ?
O2 C5 C6 120.0(7) . . ?
F7A C6 F8A 109.1(13) . . ?
F7 C6 F9 99.4(10) . . ?
F7 C6 F8 91.2(11) . . ?
F9 C6 F8 94.9(9) . . ?
F7A C6 F9A 97.3(12) . . ?
F8A C6 F9A 99.5(11) . . ?
F7A C6 C5 116.8(11) . . ?
F8A C6 C5 121.8(12) . . ?
F7 C6 C5 120.7(9) . . ?
F9 C6 C5 119.6(11) . . ?
F8 C6 C5 124.4(9) . . ?
F9A C6 C5 107.7(10) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 P1 122.0(3) . . ?
C16 C11 P1 117.6(3) . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C11 120.0 . . ?
C22 C21 C26 120.0 . . ?
C22 C21 P1 117.2(3) . . ?
C26 C21 P1 122.7(3) . . ?
C21 C22 C23 120.0 . . ?
C24 C23 C22 120.0 . . ?
C25 C24 C23 120.0 . . ?
C24 C25 C26 120.0 . . ?
C25 C26 C21 120.0 . . ?
C32 C31 C36 120.0 . . ?
C32 C31 P2 115.7(3) . . ?
C36 C31 P2 123.9(3) . . ?
C31 C32 C33 120.0 . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C31 120.0 . . ?
C42 C41 C46 120.0 . . ?
C42 C41 P2 112.5(3) . . ?
C46 C41 P2 127.4(3) . . ?
C41 C42 C43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C45 C44 C43 120.0 . . ?
C44 C45 C46 120.0 . . ?
C45 C46 C41 120.0 . . ?
C52 C51 C56 120.0 . . ?
C52 C51 P3 125.3(3) . . ?
C56 C51 P3 114.5(3) . . ?
C53 C52 C51 120.0 . . ?
C52 C53 C54 120.0 . . ?
C53 C54 C55 120.0 . . ?
C56 C55 C54 120.0 . . ?
C55 C56 C51 120.0 . . ?
C62 C61 C66 120.0 . . ?
C62 C61 P3 113.9(3) . . ?
C66 C61 P3 125.9(3) . . ?
C61 C62 C63 120.0 . . ?
C64 C63 C62 120.0 . . ?
C65 C64 C63 120.0 . . ?
C66 C65 C64 120.0 . . ?
C65 C66 C61 120.0 . . ?
C72 C71 C76 120.0 . . ?
C72 C71 P4 117.6(3) . . ?
C76 C71 P4 122.4(3) . . ?
C71 C72 C73 120.0 . . ?
C74 C73 C72 120.0 . . ?
C75 C74 C73 120.0 . . ?
C76 C75 C74 120.0 . . ?
C75 C76 C71 120.0 . . ?
C82 C81 C86 120.0 . . ?
C82 C81 P4 128.4(3) . . ?
C86 C81 P4 111.5(3) . . ?
C83 C82 C81 120.0 . . ?
C82 C83 C84 120.0 . . ?
C83 C84 C85 120.0 . . ?
C86 C85 C84 120.0 . . ?
C85 C86 C81 120.0 . . ?
O1 N1 Tc1 179.1(5) . . ?
C5 O2 Tc1 131.9(6) . . ?
C11 P1 C1 110.2(3) . . ?
C11 P1 C21 97.9(3) . . ?
C1 P1 C21 104.8(3) . . ?
C11 P1 Tc1 122.4(2) . . ?
C1 P1 Tc1 101.4(2) . . ?
C21 P1 Tc1 119.13(14) . . ?
C31 P2 C2 93.7(3) . . ?
C31 P2 C41 109.4(3) . . ?
C2 P2 C41 116.9(3) . . ?
C31 P2 Tc1 118.37(19) . . ?
C2 P2 Tc1 104.3(3) . . ?
C41 P2 Tc1 112.97(19) . . ?
C61 P3 C3 111.1(3) . . ?
C61 P3 C51 109.8(3) . . ?
C3 P3 C51 98.8(3) . . ?
C61 P3 Tc1 104.1(2) . . ?
C3 P3 Tc1 105.7(2) . . ?
C51 P3 Tc1 126.79(16) . . ?
C4 P4 C81 95.0(4) . . ?
C4 P4 C71 106.2(3) . . ?
C81 P4 C71 111.7(3) . . ?
C4 P4 Tc1 105.7(3) . . ?
C81 P4 Tc1 118.4(2) . . ?
C71 P4 Tc1 116.50(18) . . ?
F6 P5 F3 177.1(5) . . ?
F6 P5 F1 91.9(5) . . ?
F3 P5 F1 89.6(4) . . ?
F6 P5 F4 88.8(4) . . ?
F3 P5 F4 89.6(4) . . ?
F1 P5 F4 179.3(5) . . ?
F6 P5 F2 84.5(4) . . ?
F3 P5 F2 98.0(3) . . ?
F1 P5 F2 92.4(5) . . ?
F4 P5 F2 87.8(4) . . ?
F6 P5 F5 96.4(4) . . ?
F3 P5 F5 81.1(3) . . ?
F1 P5 F5 88.7(5) . . ?
F4 P5 F5 91.2(5) . . ?
F2 P5 F5 178.6(4) . . ?
N1 Tc1 O2 172.0(2) . . ?
N1 Tc1 P3 101.79(17) . . ?
O2 Tc1 P3 70.21(13) . . ?
N1 Tc1 P1 80.01(17) . . ?
O2 Tc1 P1 108.00(13) . . ?
P3 Tc1 P1 178.20(8) . . ?
N1 Tc1 P2 92.2(2) . . ?
O2 Tc1 P2 89.64(15) . . ?
P3 Tc1 P2 97.12(7) . . ?
P1 Tc1 P2 82.68(7) . . ?
N1 Tc1 P4 94.5(2) . . ?
O2 Tc1 P4 83.86(15) . . ?
P3 Tc1 P4 82.41(7) . . ?
P1 Tc1 P4 97.57(7) . . ?
P2 Tc1 P4 173.25(7) . . ?

_refine_diff_density_max         1.134
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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_tcnof4h2o
_database_code_depnum_ccdc_archive 'CCDC 1564387'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT03084C 2017
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-05-14 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         'Cs,  F4 N O2 H2 Tc'
_chemical_formula_sum            'Cs F4 H2 N O2 Tc'
_chemical_formula_weight         354.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cs Cs -0.3680 2.1192 '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'
Tc Tc -1.4390 0.7593 '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'

_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                   13.312(2)
_cell_length_b                   6.7100(10)
_cell_length_c                   17.235(2)
_cell_angle_alpha                90
_cell_angle_beta                 120.920(10)
_cell_angle_gamma                90
_cell_volume                     1320.7(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    7019
_cell_measurement_theta_min      3.43
_cell_measurement_theta_max      29.50

_exptl_crystal_description       block
_exptl_crystal_colour            Pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.570
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    7.627
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.4214
_exptl_absorpt_correction_T_max  0.6562
_exptl_absorpt_process_details   
;
P. Coppens in "Crystallographic Computing" ed F.R Ahmed, S.R. Hall 
and C.P.Huber, Copenhagen, Munksgaard, (1979) pp 255-270
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            7115
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.334
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2585
_reflns_number_gt                1767
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    Shlexs97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  WINGX
_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)+(0.0230P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2585
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0545
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_restrained_S_all      0.921
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc4 Tc 0.25277(6) -0.25839(11) -0.02262(4) 0.02225(15) Uani 1 1 d . . . . .
F1 F 0.0925(4) -0.2383(8) -0.1226(3) 0.0323(11) Uani 1 1 d . . . . .
F2 F 0.2820(5) 0.0272(7) -0.0328(3) 0.0307(12) Uani 1 1 d . . . . .
F3 F 0.2425(5) -0.5452(7) -0.0255(3) 0.0347(12) Uani 1 1 d . . . . .
F4 F 0.4224(4) -0.2856(10) 0.0613(3) 0.0471(14) Uani 1 1 d . . . . .
O1 O 0.1784(6) -0.2066(12) 0.1074(4) 0.0480(18) Uani 1 1 d . . . . .
O2 O 0.2891(5) -0.2927(9) -0.1289(3) 0.0295(13) Uani 1 1 d . . . . .
H1O2 H 0.2775 -0.3884 -0.1657 0.035 Uiso 1 1 d . U . . .
H2O2 H 0.2779 -0.1845 -0.1592 0.035 Uiso 1 1 d . U . . .
N1 N 0.2144(6) -0.2283(12) 0.0583(4) 0.0293(16) Uani 1 1 d . . . . .
Tc1 Tc 0.25363(6) -0.78908(10) -0.26625(4) 0.02033(14) Uani 1 1 d . . . . .
F5 F 0.1723(5) -0.5880(7) -0.2344(3) 0.0327(12) Uani 1 1 d . . . . .
F6 F 0.1695(4) -1.0008(7) -0.2427(3) 0.0284(11) Uani 1 1 d . . . . .
F7 F 0.3596(5) -0.5857(7) -0.2616(3) 0.0314(12) Uani 1 1 d . . . . .
F8 F 0.3526(5) -0.9878(8) -0.2743(4) 0.0345(12) Uani 1 1 d . . . . .
O3 O 0.0812(5) -0.7643(14) -0.4577(3) 0.060(2) Uani 1 1 d . . . . .
O4 O 0.3669(5) -0.8075(12) -0.1255(4) 0.0454(19) Uani 1 1 d . . . . .
H1O4 H 0.3457 -0.8005 -0.0866 0.050 Uiso 1 1 d . . . . .
H2O4 H 0.4418 -0.8192 -0.0956 0.050 Uiso 1 1 d . . . . .
N2 N 0.1548(6) -0.7770(12) -0.3802(4) 0.0289(15) Uani 1 1 d . . . . .
Cs1 Cs 0.53127(4) -0.27371(9) -0.13788(3) 0.02776(14) Uani 1 1 d . . . . .
Cs2 Cs -0.03417(4) -0.28427(9) -0.34072(3) 0.02578(13) 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
Tc4 N1 1.726(6) . ?
Tc4 F3 1.928(5) . ?
Tc4 F1 1.939(4) . ?
Tc4 F4 1.967(5) . ?
Tc4 F2 1.981(5) . ?
Tc4 O2 2.134(4) . ?
Tc4 Cs2 4.1344(10) 2_554 ?
Tc4 Cs1 4.1953(10) 3_645 ?
Tc4 Cs2 4.4072(11) 2_544 ?
F1 Cs2 3.127(5) 2_554 ?
F1 Cs2 3.250(4) . ?
F1 Cs2 3.731(5) 2_544 ?
F2 Cs2 3.137(5) 2_554 ?
F2 Cs1 3.171(5) 3_655 ?
F3 Cs2 3.001(5) 2_544 ?
F3 Cs1 3.125(5) 3_645 ?
F4 Cs1 3.167(6) 3_645 ?
O1 N1 1.175(7) . ?
O1 Cs2 3.379(6) 4_556 ?
O2 Cs1 3.308(5) . ?
O2 H1O2 0.8590 . ?
O2 H2O2 0.8606 . ?
Tc1 N2 1.715(6) . ?
Tc1 F8 1.928(5) . ?
Tc1 F7 1.935(5) . ?
Tc1 F6 1.976(5) . ?
Tc1 F5 1.976(5) . ?
Tc1 O4 2.101(5) . ?
Tc1 Cs1 3.9753(9) 2_644 ?
Tc1 Cs2 4.1796(9) 2_544 ?
F5 Cs2 3.039(5) 2_544 ?
F5 Cs2 3.144(5) . ?
F6 Cs2 3.019(5) 1_545 ?
F6 Cs2 3.176(5) 2_544 ?
F7 Cs1 3.024(5) . ?
F7 Cs1 3.048(4) 2_644 ?
F8 Cs1 3.020(5) 1_545 ?
F8 Cs1 3.025(5) 2_644 ?
O3 N2 1.185(8) . ?
O3 Cs2 3.215(5) 3_544 ?
O4 H1O4 0.8520 . ?
O4 H2O4 0.8598 . ?
Cs1 F8 3.020(5) 1_565 ?
Cs1 F8 3.025(5) 2_654 ?
Cs1 F7 3.048(4) 2_654 ?
Cs1 F3 3.125(5) 3_645 ?
Cs1 F4 3.167(6) 3_645 ?
Cs1 F2 3.171(5) 3_655 ?
Cs1 Tc1 3.9754(9) 2_654 ?
Cs1 Tc4 4.1954(10) 3_645 ?
Cs1 Cs1 4.8559(8) 2_654 ?
Cs1 Cs1 4.8559(8) 2_644 ?
Cs1 H1O2 3.2505 . ?
Cs1 H2O2 3.2561 . ?
Cs2 F3 3.001(5) 2_554 ?
Cs2 F6 3.019(5) 1_565 ?
Cs2 F5 3.039(5) 2_554 ?
Cs2 F1 3.127(5) 2_544 ?
Cs2 F2 3.137(5) 2_544 ?
Cs2 F6 3.176(5) 2_554 ?
Cs2 O3 3.215(5) 3_544 ?
Cs2 O1 3.379(6) 4 ?
Cs2 F1 3.731(5) 2_554 ?
Cs2 Tc4 4.1343(10) 2_544 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Tc4 F3 95.2(3) . . ?
N1 Tc4 F1 93.5(3) . . ?
F3 Tc4 F1 90.9(2) . . ?
N1 Tc4 F4 97.0(3) . . ?
F3 Tc4 F4 88.1(3) . . ?
F1 Tc4 F4 169.48(18) . . ?
N1 Tc4 F2 96.4(3) . . ?
F3 Tc4 F2 167.9(2) . . ?
F1 Tc4 F2 91.7(2) . . ?
F4 Tc4 F2 87.2(2) . . ?
N1 Tc4 O2 176.5(3) . . ?
F3 Tc4 O2 85.1(2) . . ?
F1 Tc4 O2 82.91(19) . . ?
F4 Tc4 O2 86.6(2) . . ?
F2 Tc4 O2 83.5(2) . . ?
N1 Tc4 Cs2 87.5(3) . 2_554 ?
F3 Tc4 Cs2 137.16(17) . 2_554 ?
F1 Tc4 Cs2 46.32(16) . 2_554 ?
F4 Tc4 Cs2 134.14(19) . 2_554 ?
F2 Tc4 Cs2 46.98(15) . 2_554 ?
O2 Tc4 Cs2 89.87(16) . 2_554 ?
N1 Tc4 Cs1 86.7(3) . 3_645 ?
F3 Tc4 Cs1 44.42(16) . 3_645 ?
F1 Tc4 Cs1 134.92(16) . 3_645 ?
F4 Tc4 Cs1 46.11(18) . 3_645 ?
F2 Tc4 Cs1 133.10(15) . 3_645 ?
O2 Tc4 Cs1 95.99(16) . 3_645 ?
Cs2 Tc4 Cs1 174.112(17) 2_554 3_645 ?
N1 Tc4 Cs2 97.9(3) . 2_544 ?
F3 Tc4 Cs2 33.73(16) . 2_544 ?
F1 Tc4 Cs2 57.18(16) . 2_544 ?
F4 Tc4 Cs2 120.80(19) . 2_544 ?
F2 Tc4 Cs2 146.38(14) . 2_544 ?
O2 Tc4 Cs2 80.42(16) . 2_544 ?
Cs2 Tc4 Cs2 103.50(2) 2_554 2_544 ?
Cs1 Tc4 Cs2 78.10(2) 3_645 2_544 ?
Tc4 F1 Cs2 107.0(2) . 2_554 ?
Tc4 F1 Cs2 134.49(17) . . ?
Cs2 F1 Cs2 86.05(11) 2_554 . ?
Tc4 F1 Cs2 96.91(18) . 2_544 ?
Cs2 F1 Cs2 156.05(14) 2_554 2_544 ?
Cs2 F1 Cs2 76.79(10) . 2_544 ?
Tc4 F2 Cs2 105.5(2) . 2_554 ?
Tc4 F2 Cs1 121.20(19) . 3_655 ?
Cs2 F2 Cs1 118.52(15) 2_554 3_655 ?
Tc4 F3 Cs2 125.4(2) . 2_544 ?
Tc4 F3 Cs1 110.0(2) . 3_645 ?
Cs2 F3 Cs1 124.53(16) 2_544 3_645 ?
Tc4 F4 Cs1 107.3(2) . 3_645 ?
N1 O1 Cs2 153.4(6) . 4_556 ?
Tc4 O2 Cs1 133.8(2) . . ?
Tc4 O2 H1O2 132.9 . . ?
Cs1 O2 H1O2 78.7 . . ?
Tc4 O2 H2O2 112.5 . . ?
Cs1 O2 H2O2 79.1 . . ?
H1O2 O2 H2O2 105.9 . . ?
O1 N1 Tc4 174.2(6) . . ?
N2 Tc1 F8 95.8(3) . . ?
N2 Tc1 F7 97.4(3) . . ?
F8 Tc1 F7 88.9(2) . . ?
N2 Tc1 F6 95.0(3) . . ?
F8 Tc1 F6 89.9(2) . . ?
F7 Tc1 F6 167.64(19) . . ?
N2 Tc1 F5 94.5(3) . . ?
F8 Tc1 F5 169.7(2) . . ?
F7 Tc1 F5 89.9(2) . . ?
F6 Tc1 F5 89.13(19) . . ?
N2 Tc1 O4 176.8(3) . . ?
F8 Tc1 O4 86.0(3) . . ?
F7 Tc1 O4 85.3(2) . . ?
F6 Tc1 O4 82.3(2) . . ?
F5 Tc1 O4 83.7(3) . . ?
N2 Tc1 Cs1 79.4(2) . 2_644 ?
F8 Tc1 Cs1 47.45(14) . 2_644 ?
F7 Tc1 Cs1 48.18(14) . 2_644 ?
F6 Tc1 Cs1 135.18(14) . 2_644 ?
F5 Tc1 Cs1 135.41(15) . 2_644 ?
O4 Tc1 Cs1 103.81(15) . 2_644 ?
N2 Tc1 Cs2 101.9(2) . 2_544 ?
F8 Tc1 Cs2 134.02(14) . 2_544 ?
F7 Tc1 Cs2 129.52(14) . 2_544 ?
F6 Tc1 Cs2 46.89(14) . 2_544 ?
F5 Tc1 Cs2 42.72(14) . 2_544 ?
O4 Tc1 Cs2 74.96(15) . 2_544 ?
Cs1 Tc1 Cs2 177.65(2) 2_644 2_544 ?
Tc1 F5 Cs2 111.1(2) . 2_544 ?
Tc1 F5 Cs2 136.1(2) . . ?
Cs2 F5 Cs2 89.44(14) 2_544 . ?
Tc1 F6 Cs2 141.1(2) . 1_545 ?
Tc1 F6 Cs2 106.09(19) . 2_544 ?
Cs2 F6 Cs2 89.21(13) 1_545 2_544 ?
Tc1 F7 Cs1 142.04(19) . . ?
Tc1 F7 Cs1 103.58(19) . 2_644 ?
Cs1 F7 Cs1 106.21(15) . 2_644 ?
Tc1 F8 Cs1 132.6(2) . 1_545 ?
Tc1 F8 Cs1 104.5(2) . 2_644 ?
Cs1 F8 Cs1 106.89(16) 1_545 2_644 ?
N2 O3 Cs2 144.5(5) . 3_544 ?
Tc1 O4 H1O4 125.0 . . ?
Tc1 O4 H2O4 128.3 . . ?
H1O4 O4 H2O4 106.6 . . ?
O3 N2 Tc1 175.7(6) . . ?
F8 Cs1 F7 83.30(14) 1_565 . ?
F8 Cs1 F8 108.23(9) 1_565 2_654 ?
F7 Cs1 F8 73.37(12) . 2_654 ?
F8 Cs1 F7 73.11(12) 1_565 2_654 ?
F7 Cs1 F7 107.09(9) . 2_654 ?
F8 Cs1 F7 52.88(13) 2_654 2_654 ?
F8 Cs1 F3 163.27(14) 1_565 3_645 ?
F7 Cs1 F3 113.30(14) . 3_645 ?
F8 Cs1 F3 76.27(14) 2_654 3_645 ?
F7 Cs1 F3 98.81(13) 2_654 3_645 ?
F8 Cs1 F4 145.52(14) 1_565 3_645 ?
F7 Cs1 F4 64.02(14) . 3_645 ?
F8 Cs1 F4 74.04(14) 2_654 3_645 ?
F7 Cs1 F4 125.15(13) 2_654 3_645 ?
F3 Cs1 F4 50.97(12) 3_645 3_645 ?
F8 Cs1 F2 108.63(14) 1_565 3_655 ?
F7 Cs1 F2 164.46(12) . 3_655 ?
F8 Cs1 F2 110.69(14) 2_654 3_655 ?
F7 Cs1 F2 86.34(12) 2_654 3_655 ?
F3 Cs1 F2 55.49(13) 3_645 3_655 ?
F4 Cs1 F2 102.04(13) 3_645 3_655 ?
F8 Cs1 O2 70.37(14) 1_565 . ?
F7 Cs1 O2 66.72(13) . . ?
F8 Cs1 O2 139.99(14) 2_654 . ?
F7 Cs1 O2 143.41(14) 2_654 . ?
F3 Cs1 O2 117.01(13) 3_645 . ?
F4 Cs1 O2 86.00(14) 3_645 . ?
F2 Cs1 O2 107.16(13) 3_655 . ?
F8 Cs1 Tc1 98.07(9) 1_565 2_654 ?
F7 Cs1 Tc1 97.68(8) . 2_654 ?
F8 Cs1 Tc1 28.00(10) 2_654 2_654 ?
F7 Cs1 Tc1 28.23(9) 2_654 2_654 ?
F3 Cs1 Tc1 78.34(9) 3_645 2_654 ?
F4 Cs1 Tc1 96.97(9) 3_645 2_654 ?
F2 Cs1 Tc1 90.60(8) 3_655 2_654 ?
O2 Cs1 Tc1 161.03(9) . 2_654 ?
F8 Cs1 Tc4 170.94(11) 1_565 3_645 ?
F7 Cs1 Tc4 87.73(10) . 3_645 ?
F8 Cs1 Tc4 67.75(11) 2_654 3_645 ?
F7 Cs1 Tc4 108.62(10) 2_654 3_645 ?
F3 Cs1 Tc4 25.59(9) 3_645 3_645 ?
F4 Cs1 Tc4 26.60(9) 3_645 3_645 ?
F2 Cs1 Tc4 80.42(9) 3_655 3_645 ?
O2 Cs1 Tc4 107.12(10) . 3_645 ?
Tc1 Cs1 Tc4 81.879(18) 2_654 3_645 ?
F8 Cs1 Cs1 36.60(9) 1_565 2_654 ?
F7 Cs1 Cs1 99.14(9) . 2_654 ?
F8 Cs1 Cs1 81.51(10) 2_654 2_654 ?
F7 Cs1 Cs1 36.72(10) 2_654 2_654 ?
F3 Cs1 Cs1 132.66(9) 3_645 2_654 ?
F4 Cs1 Cs1 153.35(10) 3_645 2_654 ?
F2 Cs1 Cs1 96.33(8) 3_655 2_654 ?
O2 Cs1 Cs1 106.92(10) . 2_654 ?
Tc1 Cs1 Cs1 63.423(17) 2_654 2_654 ?
Tc4 Cs1 Cs1 145.182(18) 3_645 2_654 ?
F8 Cs1 Cs1 94.30(10) 1_565 2_644 ?
F7 Cs1 Cs1 37.07(9) . 2_644 ?
F8 Cs1 Cs1 36.52(11) 2_654 2_644 ?
F7 Cs1 Cs1 76.72(9) 2_654 2_644 ?
F3 Cs1 Cs1 98.07(9) 3_645 2_644 ?
F4 Cs1 Cs1 66.64(10) 3_645 2_644 ?
F2 Cs1 Cs1 146.19(9) 3_655 2_644 ?
O2 Cs1 Cs1 103.76(10) . 2_644 ?
Tc1 Cs1 Cs1 61.103(16) 2_654 2_644 ?
Tc4 Cs1 Cs1 77.695(16) 3_645 2_644 ?
Cs1 Cs1 Cs1 87.405(18) 2_654 2_644 ?
F8 Cs1 H1O2 72.1 1_565 . ?
F7 Cs1 H1O2 51.7 . . ?
F8 Cs1 H1O2 125.0 2_654 . ?
F7 Cs1 H1O2 141.0 2_654 . ?
F3 Cs1 H1O2 119.2 3_645 . ?
F4 Cs1 H1O2 78.8 3_645 . ?
F2 Cs1 H1O2 121.4 3_655 . ?
O2 Cs1 H1O2 15.0 . . ?
Tc1 Cs1 H1O2 148.0 2_654 . ?
Tc4 Cs1 H1O2 103.2 3_645 . ?
Cs1 Cs1 H1O2 107.8 2_654 . ?
Cs1 Cs1 H1O2 88.8 2_644 . ?
F8 Cs1 H2O2 55.9 1_565 . ?
F7 Cs1 H2O2 71.6 . . ?
F8 Cs1 H2O2 142.9 2_654 . ?
F7 Cs1 H2O2 129.0 2_654 . ?
F3 Cs1 H2O2 129.5 3_645 . ?
F4 Cs1 H2O2 100.8 3_645 . ?
F2 Cs1 H2O2 106.4 3_655 . ?
O2 Cs1 H2O2 15.0 . . ?
Tc1 Cs1 H2O2 152.1 2_654 . ?
Tc4 Cs1 H2O2 122.1 3_645 . ?
Cs1 Cs1 H2O2 92.3 2_654 . ?
Cs1 Cs1 H2O2 107.1 2_644 . ?
H1O2 Cs1 H2O2 24.4 . . ?
F3 Cs2 F6 107.62(14) 2_554 1_565 ?
F3 Cs2 F5 64.74(13) 2_554 2_554 ?
F6 Cs2 F5 93.12(13) 1_565 2_554 ?
F3 Cs2 F1 109.27(13) 2_554 2_544 ?
F6 Cs2 F1 141.73(13) 1_565 2_544 ?
F5 Cs2 F1 111.52(12) 2_554 2_544 ?
F3 Cs2 F2 56.99(14) 2_554 2_544 ?
F6 Cs2 F2 164.59(13) 1_565 2_544 ?
F5 Cs2 F2 79.66(13) 2_554 2_544 ?
F1 Cs2 F2 53.39(12) 2_544 2_544 ?
F3 Cs2 F5 168.48(12) 2_554 . ?
F6 Cs2 F5 79.48(12) 1_565 . ?
F5 Cs2 F5 124.85(8) 2_554 . ?
F1 Cs2 F5 62.50(12) 2_544 . ?
F2 Cs2 F5 115.82(13) 2_544 . ?
F3 Cs2 F6 94.42(13) 2_554 2_554 ?
F6 Cs2 F6 126.17(8) 1_565 2_554 ?
F5 Cs2 F6 52.94(12) 2_554 2_554 ?
F1 Cs2 F6 60.42(11) 2_544 2_554 ?
F2 Cs2 F6 59.43(12) 2_544 2_554 ?
F5 Cs2 F6 88.22(12) . 2_554 ?
F3 Cs2 O3 61.69(16) 2_554 3_544 ?
F6 Cs2 O3 99.27(16) 1_565 3_544 ?
F5 Cs2 O3 126.30(17) 2_554 3_544 ?
F1 Cs2 O3 89.41(18) 2_544 3_544 ?
F2 Cs2 O3 74.86(15) 2_544 3_544 ?
F5 Cs2 O3 108.78(16) . 3_544 ?
F6 Cs2 O3 134.02(16) 2_554 3_544 ?
F3 Cs2 F1 124.28(12) 2_554 . ?
F6 Cs2 F1 60.66(11) 1_565 . ?
F5 Cs2 F1 62.20(13) 2_554 . ?
F1 Cs2 F1 104.71(13) 2_544 . ?
F2 Cs2 F1 125.25(11) 2_544 . ?
F5 Cs2 F1 66.98(12) . . ?
F6 Cs2 F1 66.26(12) 2_554 . ?
O3 Cs2 F1 159.72(16) 3_544 . ?
F3 Cs2 O1 112.05(15) 2_554 4 ?
F6 Cs2 O1 61.71(15) 1_565 4 ?
F5 Cs2 O1 153.25(16) 2_554 4 ?
F1 Cs2 O1 94.77(15) 2_544 4 ?
F2 Cs2 O1 122.25(14) 2_544 4 ?
F5 Cs2 O1 62.76(15) . 4 ?
F6 Cs2 O1 149.18(16) 2_554 4 ?
O3 Cs2 O1 55.95(16) 3_544 4 ?
F1 Cs2 O1 107.52(13) . 4 ?
F3 Cs2 F1 46.79(12) 2_554 2_554 ?
F6 Cs2 F1 61.65(12) 1_565 2_554 ?
F5 Cs2 F1 61.84(11) 2_554 2_554 ?
F1 Cs2 F1 156.05(14) 2_544 2_554 ?
F2 Cs2 F1 103.02(11) 2_544 2_554 ?
F5 Cs2 F1 141.13(12) . 2_554 ?
F6 Cs2 F1 114.15(10) 2_554 2_554 ?
O3 Cs2 F1 79.00(18) 3_544 2_554 ?
F1 Cs2 F1 92.41(12) . 2_554 ?
O1 Cs2 F1 95.88(15) 4 2_554 ?
F3 Cs2 Tc4 82.63(10) 2_554 2_544 ?
F6 Cs2 Tc4 166.01(10) 1_565 2_544 ?
F5 Cs2 Tc4 99.99(10) 2_554 2_544 ?
F1 Cs2 Tc4 26.65(8) 2_544 2_544 ?
F2 Cs2 Tc4 27.50(9) 2_544 2_544 ?
F5 Cs2 Tc4 88.96(10) . 2_544 ?
F6 Cs2 Tc4 60.58(8) 2_554 2_544 ?
O3 Cs2 Tc4 76.88(16) 3_544 2_544 ?
F1 Cs2 Tc4 121.81(9) . 2_544 ?
O1 Cs2 Tc4 105.98(13) 4 2_544 ?
F1 Cs2 Tc4 129.40(7) 2_554 2_544 ?


loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H1O2 F5 0.86 1.86 2.597(8) 143.1 .
O2 H2O2 F6 0.86 1.88 2.647(8) 147.5 1_565
O4 H1O4 F2 0.85 1.93 2.629(7) 138.6 1_545
O4 H2O4 F4 0.86 1.74 2.508(7) 148.4 3_645

_refine_diff_density_max         0.758
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.170

####################################################################### 
# 
# 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_cstcnopph3tfa
_audit_block_doi                 10.5517/ccdc.csd.cc1phw46
_database_code_depnum_ccdc_archive 'CCDC 1564388'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7DT03084C 2017
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-05-14 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT601_cstcnopph3tfa       
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        738 Ang3  
RESPONSE:The VOIDS result from the arrangement of cation and anion. 
;
_vrf_RINTA01_cstcnopph3tfa       
;
PROBLEM:  The value of Rint is greater than 0.18
RESPONSE:  It arises from the limited quality of the crystals. 
;
_vrf_PLAT020_cstcnopph3tfa       
;
PROBLEM: The value of Rint is greater than 0.12  
RESPONSE:  It arises from the limited quality of the crystals. 
;
_vrf_PLAT342_cstcnopph3tfa       
;
PROBLEM: Low Bond Precision on  C-C Bonds 
RESPONSE:It arises from the limited quality of the crystals.  
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H30 F7 N O5 P2 Tc, Cs'
_chemical_formula_sum            'C40 H30 Cs F7 N O5 P2 Tc'
_chemical_formula_weight         1030.50

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_H-M_alt        'I -4 c 2'
_space_group_name_Hall           'I -4 -2c'

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

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

_cell_length_a                   24.8130(10)
_cell_length_b                   24.8130(10)
_cell_length_c                   28.394(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17481.8(19)
_cell_formula_units_Z            16
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    12346
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      43.19

_exptl_crystal_description       needle
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_F_000             8128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.294
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            46256
_diffrn_reflns_av_unetI/netI     0.2090
_diffrn_reflns_av_R_equivalents  0.2375
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.845
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7691
_reflns_number_gt                3684
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

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

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  WingX
_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)+(0.0727P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1095 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7691
_refine_ls_number_parameters     431
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.1549
_refine_ls_R_factor_gt           0.0766
_refine_ls_wR_factor_ref         0.1842
_refine_ls_wR_factor_gt          0.1547
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_restrained_S_all      0.874
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8374(9) 0.2455(9) 0.1154(9) 0.040(4) Uani 1 1 d . . . . .
C2 C 0.8527(15) 0.2960(11) 0.1388(12) 0.084(7) Uani 1 1 d . U . . .
C3 C 0.6978(8) 0.2345(9) 0.1312(9) 0.040(4) Uani 1 1 d . . . . .
C4 C 0.6599(18) 0.2723(19) 0.1551(15) 0.118(8) Uani 1 1 d . U . . .
C11 C 0.6917(6) 0.0302(6) 0.1715(4) 0.028(5) Uani 1 1 d G . . . .
C12 C 0.6907(7) -0.0257(6) 0.1693(6) 0.080(9) Uani 1 1 d G . . . .
H12 H 0.6949 -0.0431 0.1405 0.096 Uiso 1 1 calc R U . . .
C13 C 0.6835(8) -0.0557(5) 0.2102(8) 0.080(9) Uani 1 1 d G . . . .
H13 H 0.6828 -0.0931 0.2088 0.096 Uiso 1 1 calc R U . . .
C14 C 0.6773(7) -0.0297(8) 0.2532(6) 0.089(9) Uani 1 1 d G . . . .
H14 H 0.6725 -0.0498 0.2806 0.107 Uiso 1 1 calc R U . . .
C15 C 0.6783(7) 0.0262(8) 0.2554(4) 0.068(8) Uani 1 1 d G . . . .
H15 H 0.6742 0.0436 0.2842 0.081 Uiso 1 1 calc R U . . .
C16 C 0.6855(6) 0.0562(5) 0.2145(5) 0.053(6) Uani 1 1 d G . . . .
H16 H 0.6862 0.0936 0.2160 0.063 Uiso 1 1 calc R U . . .
C21 C 0.7031(6) 0.0219(6) 0.0705(5) 0.039(3) Uani 1 1 d G U . . .
C22 C 0.6580(5) -0.0094(7) 0.0610(6) 0.074(9) Uani 1 1 d G U . . .
H22 H 0.6264 -0.0043 0.0781 0.089 Uiso 1 1 calc R U . . .
C23 C 0.6600(6) -0.0485(7) 0.0260(6) 0.079(9) Uani 1 1 d G U . . .
H23 H 0.6298 -0.0695 0.0196 0.095 Uiso 1 1 calc R U . . .
C24 C 0.7072(7) -0.0562(6) 0.0004(5) 0.068(7) Uani 1 1 d G U . . .
H24 H 0.7086 -0.0824 -0.0230 0.082 Uiso 1 1 calc R U . . .
C25 C 0.7523(6) -0.0249(6) 0.0099(5) 0.057(6) Uani 1 1 d G U . . .
H25 H 0.7839 -0.0300 -0.0071 0.069 Uiso 1 1 calc R U . . .
C26 C 0.7503(5) 0.0142(6) 0.0450(6) 0.051(6) Uani 1 1 d G U . . .
H26 H 0.7805 0.0352 0.0513 0.061 Uiso 1 1 calc R U . . .
C31 C 0.6351(5) 0.1047(6) 0.1091(5) 0.039(3) Uani 1 1 d G U . . .
C32 C 0.6310(5) 0.1402(7) 0.0714(5) 0.060(6) Uani 1 1 d G U . . .
H32 H 0.6605 0.1462 0.0519 0.072 Uiso 1 1 calc R U . . .
C33 C 0.5826(6) 0.1667(7) 0.0628(5) 0.070(8) Uani 1 1 d G U . . .
H33 H 0.5798 0.1905 0.0375 0.084 Uiso 1 1 calc R U . . .
C34 C 0.5384(5) 0.1578(8) 0.0918(6) 0.082(9) Uani 1 1 d G U . . .
H34 H 0.5061 0.1755 0.0861 0.098 Uiso 1 1 calc R U . . .
C35 C 0.5426(5) 0.1223(8) 0.1295(6) 0.082(8) Uani 1 1 d G U . . .
H35 H 0.5131 0.1163 0.1490 0.099 Uiso 1 1 calc R U . . .
C36 C 0.5910(6) 0.0958(7) 0.1381(5) 0.063(6) Uani 1 1 d G U . . .
H36 H 0.5938 0.0720 0.1634 0.075 Uiso 1 1 calc R U . . .
C41 C 0.8697(5) 0.0264(4) 0.1418(5) 0.035(5) Uani 1 1 d G U . . .
C42 C 0.8264(4) -0.0053(6) 0.1557(7) 0.065(8) Uani 1 1 d G U . . .
H42 H 0.7913 0.0062 0.1501 0.078 Uiso 1 1 calc R U . . .
C43 C 0.8355(5) -0.0544(6) 0.1779(8) 0.105(14) Uani 1 1 d G U . . .
H43 H 0.8065 -0.0757 0.1872 0.126 Uiso 1 1 calc R U . . .
C44 C 0.8879(6) -0.0717(5) 0.1863(6) 0.055(6) Uani 1 1 d G U . . .
H44 H 0.8940 -0.1045 0.2012 0.066 Uiso 1 1 calc R U . . .
C45 C 0.9312(5) -0.0399(6) 0.1724(6) 0.062(7) Uani 1 1 d G U . . .
H45 H 0.9663 -0.0515 0.1780 0.074 Uiso 1 1 calc R U . . .
C46 C 0.9221(5) 0.0092(6) 0.1502(6) 0.063(7) Uani 1 1 d G U . . .
H46 H 0.9511 0.0304 0.1409 0.075 Uiso 1 1 calc R U . . .
C51 C 0.8761(6) 0.0827(5) 0.0524(3) 0.033(5) Uani 1 1 d G U . . .
C52 C 0.8898(5) 0.0321(4) 0.0352(4) 0.035(5) Uani 1 1 d G U . . .
H52 H 0.8919 0.0029 0.0556 0.042 Uiso 1 1 calc R U . . .
C53 C 0.9002(5) 0.0252(4) -0.0125(4) 0.043(5) Uani 1 1 d G U . . .
H53 H 0.9094 -0.0087 -0.0240 0.052 Uiso 1 1 calc R U . . .
C54 C 0.8970(6) 0.0689(5) -0.0430(3) 0.046(5) Uani 1 1 d G U . . .
H54 H 0.9040 0.0643 -0.0749 0.055 Uiso 1 1 calc R U . . .
C55 C 0.8834(5) 0.1195(5) -0.0258(4) 0.040(4) Uani 1 1 d G U . . .
H55 H 0.8812 0.1488 -0.0462 0.048 Uiso 1 1 calc R U . . .
C56 C 0.8729(5) 0.1264(4) 0.0220(4) 0.029(4) Uani 1 1 d G U . . .
H56 H 0.8637 0.1603 0.0335 0.035 Uiso 1 1 calc R U . . .
C61 C 0.9112(5) 0.1326(5) 0.1412(5) 0.034(5) Uani 1 1 d G . . . .
C62 C 0.9522(6) 0.1555(6) 0.1145(4) 0.042(6) Uani 1 1 d G . . . .
H62 H 0.9526 0.1510 0.0820 0.051 Uiso 1 1 calc R U . . .
C63 C 0.9927(5) 0.1850(6) 0.1364(5) 0.065(8) Uani 1 1 d G . . . .
H63 H 1.0201 0.2003 0.1185 0.078 Uiso 1 1 calc R U . . .
C64 C 0.9922(5) 0.1917(6) 0.1850(6) 0.059(8) Uani 1 1 d G . . . .
H64 H 1.0192 0.2115 0.1996 0.071 Uiso 1 1 calc R U . . .
C65 C 0.9512(6) 0.1688(7) 0.2117(4) 0.065(8) Uani 1 1 d G . . . .
H65 H 0.9508 0.1733 0.2442 0.078 Uiso 1 1 calc R U . . .
C66 C 0.9107(5) 0.1393(7) 0.1898(5) 0.061(7) Uani 1 1 d G . . . .
H66 H 0.8833 0.1240 0.2077 0.074 Uiso 1 1 calc R U . . .
F1 F 0.7810(4) 0.1245(4) 0.1939(4) 0.041(3) Uani 1 1 d . . . . .
F2 F 0.8249(11) 0.3371(8) 0.1226(9) 0.155(8) Uani 1 1 d . U . . .
F3 F 0.9044(9) 0.3110(9) 0.1299(8) 0.135(7) Uani 1 1 d . U . . .
F4 F 0.8495(9) 0.2993(7) 0.1845(7) 0.116(6) Uani 1 1 d . U . . .
F5 F 0.6215(11) 0.2457(10) 0.1776(10) 0.169(9) Uani 1 1 d . U . . .
F6 F 0.6834(10) 0.2973(10) 0.1896(9) 0.154(8) Uani 1 1 d . U . . .
F7 F 0.6330(8) 0.3070(9) 0.1358(9) 0.135(7) Uani 1 1 d . U . . .
N1 N 0.7624(7) 0.1476(6) 0.0637(7) 0.034(4) Uani 1 1 d . . . . .
O1 O 0.7554(6) 0.1517(7) 0.0236(6) 0.052(4) Uani 1 1 d . . . . .
O2 O 0.7088(5) 0.1919(6) 0.1500(5) 0.047(4) Uani 1 1 d . . . . .
O3 O 0.8178(6) 0.2109(5) 0.1423(5) 0.046(4) Uani 1 1 d . . . . .
O4 O 0.8467(7) 0.2413(7) 0.0737(7) 0.059(5) Uani 1 1 d . . . . .
O5 O 0.7111(8) 0.2530(7) 0.0921(7) 0.073(6) Uani 1 1 d . . . . .
P1 P 0.7019(2) 0.0716(2) 0.1187(2) 0.0342(12) Uani 1 1 d . . . . .
P2 P 0.8564(2) 0.0927(2) 0.11431(18) 0.0298(12) Uani 1 1 d . . . . .
Tc1 Tc 0.77153(7) 0.13951(7) 0.12433(6) 0.0293(4) Uani 1 1 d . . . . .
Cs1 Cs 0.77184(9) 0.27184(9) 0.0000 0.0902(9) Uani 1 2 d S T P . .
Cs2 Cs 0.78011(7) 0.21989(7) 0.2500 0.0635(7) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O4 1.21(3) . ?
C1 O3 1.25(3) . ?
C1 C2 1.47(3) . ?
C1 Cs1 3.72(2) . ?
C2 F4 1.30(3) . ?
C2 F2 1.31(4) . ?
C2 F3 1.36(4) . ?
C3 O2 1.22(2) . ?
C3 O5 1.25(3) . ?
C3 C4 1.49(4) . ?
C4 F7 1.22(4) . ?
C4 F6 1.30(5) . ?
C4 F5 1.32(5) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C11 P1 1.835(13) . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C21 P1 1.842(12) . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C31 P1 1.870(12) . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C41 P2 1.851(11) . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C51 C52 1.3900 . ?
C51 C56 1.3900 . ?
C51 P2 1.840(10) . ?
C52 C53 1.3900 . ?
C53 C54 1.3900 . ?
C54 C55 1.3900 . ?
C55 C56 1.3900 . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C61 P2 1.848(11) . ?
C62 C63 1.3900 . ?
C63 C64 1.3900 . ?
C64 C65 1.3900 . ?
C65 C66 1.3900 . ?
F1 Tc1 2.023(12) . ?
F1 Cs2 2.854(11) . ?
F4 Cs2 3.209(19) . ?
F6 Cs2 3.52(2) . ?
N1 O1 1.16(2) . ?
N1 Tc1 1.748(19) . ?
N1 Cs1 3.583(17) . ?
O1 Cs1 3.082(17) . ?
O2 Tc1 2.155(14) . ?
O2 Cs2 3.416(15) . ?
O3 Tc1 2.173(14) . ?
O3 Cs2 3.205(15) . ?
O4 Cs1 2.899(17) . ?
O5 Cs1 3.054(19) . ?
P1 Tc1 2.418(5) . ?
P2 Tc1 2.421(5) . ?
Tc1 Cs2 4.0935(19) . ?
Cs1 O4 2.899(17) 13_544 ?
Cs1 O5 3.054(19) 13_544 ?
Cs1 O1 3.082(17) 13_544 ?
Cs1 N1 3.583(17) 13_544 ?
Cs1 C1 3.72(2) 13_544 ?
Cs2 F1 2.854(11) 8_665 ?
Cs2 O3 3.205(15) 8_665 ?
Cs2 F4 3.209(19) 8_665 ?
Cs2 O2 3.416(15) 8_665 ?
Cs2 F6 3.52(2) 8_665 ?
Cs2 Tc1 4.0934(19) 8_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 C1 O3 128(2) . . ?
O4 C1 C2 118(2) . . ?
O3 C1 C2 114(2) . . ?
O4 C1 Cs1 40.2(12) . . ?
O3 C1 Cs1 119.4(14) . . ?
C2 C1 Cs1 111.2(18) . . ?
F4 C2 F2 106(3) . . ?
F4 C2 F3 103(3) . . ?
F2 C2 F3 103(3) . . ?
F4 C2 C1 119(3) . . ?
F2 C2 C1 112(3) . . ?
F3 C2 C1 113(3) . . ?
O2 C3 O5 131(2) . . ?
O2 C3 C4 119(3) . . ?
O5 C3 C4 110(3) . . ?
F7 C4 F6 104(4) . . ?
F7 C4 F5 100(3) . . ?
F6 C4 F5 101(3) . . ?
F7 C4 C3 126(4) . . ?
F6 C4 C3 111(3) . . ?
F5 C4 C3 111(4) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 P1 121.7(9) . . ?
C16 C11 P1 118.3(9) . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C14 C15 C16 120.0 . . ?
C15 C16 C11 120.0 . . ?
C22 C21 C26 120.0 . . ?
C22 C21 P1 120.4(8) . . ?
C26 C21 P1 119.5(8) . . ?
C23 C22 C21 120.0 . . ?
C22 C23 C24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C26 C25 C24 120.0 . . ?
C25 C26 C21 120.0 . . ?
C32 C31 C36 120.0 . . ?
C32 C31 P1 117.2(9) . . ?
C36 C31 P1 122.8(9) . . ?
C31 C32 C33 120.0 . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C35 120.0 . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C31 120.0 . . ?
C42 C41 C46 120.0 . . ?
C42 C41 P2 119.1(8) . . ?
C46 C41 P2 120.9(8) . . ?
C41 C42 C43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C45 C44 C43 120.0 . . ?
C46 C45 C44 120.0 . . ?
C45 C46 C41 120.0 . . ?
C52 C51 C56 120.0 . . ?
C52 C51 P2 121.5(7) . . ?
C56 C51 P2 118.3(7) . . ?
C51 C52 C53 120.0 . . ?
C54 C53 C52 120.0 . . ?
C53 C54 C55 120.0 . . ?
C54 C55 C56 120.0 . . ?
C55 C56 C51 120.0 . . ?
C62 C61 C66 120.0 . . ?
C62 C61 P2 122.2(8) . . ?
C66 C61 P2 117.8(8) . . ?
C61 C62 C63 120.0 . . ?
C64 C63 C62 120.0 . . ?
C63 C64 C65 120.0 . . ?
C66 C65 C64 120.0 . . ?
C65 C66 C61 120.0 . . ?
Tc1 F1 Cs2 113.0(5) . . ?
C2 F4 Cs2 124.8(16) . . ?
C4 F6 Cs2 114(2) . . ?
O1 N1 Tc1 178.1(18) . . ?
O1 N1 Cs1 55.7(12) . . ?
Tc1 N1 Cs1 126.0(7) . . ?
N1 O1 Cs1 106.3(14) . . ?
C3 O2 Tc1 122.5(14) . . ?
C3 O2 Cs2 107.8(14) . . ?
Tc1 O2 Cs2 91.7(5) . . ?
C1 O3 Tc1 128.5(14) . . ?
C1 O3 Cs2 130.6(13) . . ?
Tc1 O3 Cs2 97.3(5) . . ?
C1 O4 Cs1 124.2(15) . . ?
C3 O5 Cs1 161.9(16) . . ?
C11 P1 C21 103.6(7) . . ?
C11 P1 C31 104.1(7) . . ?
C21 P1 C31 101.5(7) . . ?
C11 P1 Tc1 115.7(5) . . ?
C21 P1 Tc1 120.3(5) . . ?
C31 P1 Tc1 109.7(5) . . ?
C51 P2 C61 105.7(7) . . ?
C51 P2 C41 103.6(7) . . ?
C61 P2 C41 99.8(7) . . ?
C51 P2 Tc1 114.1(5) . . ?
C61 P2 Tc1 109.6(5) . . ?
C41 P2 Tc1 122.1(5) . . ?
N1 Tc1 F1 175.9(6) . . ?
N1 Tc1 O2 99.9(7) . . ?
F1 Tc1 O2 82.2(5) . . ?
N1 Tc1 O3 101.9(7) . . ?
F1 Tc1 O3 81.9(5) . . ?
O2 Tc1 O3 79.1(6) . . ?
N1 Tc1 P1 85.5(6) . . ?
F1 Tc1 P1 91.1(4) . . ?
O2 Tc1 P1 85.8(4) . . ?
O3 Tc1 P1 164.0(4) . . ?
N1 Tc1 P2 92.9(5) . . ?
F1 Tc1 P2 85.7(3) . . ?
O2 Tc1 P2 163.1(4) . . ?
O3 Tc1 P2 87.6(4) . . ?
P1 Tc1 P2 106.23(19) . . ?
N1 Tc1 Cs2 144.1(5) . . ?
F1 Tc1 Cs2 39.9(3) . . ?
O2 Tc1 Cs2 56.5(4) . . ?
O3 Tc1 Cs2 51.0(4) . . ?
P1 Tc1 Cs2 115.75(15) . . ?
P2 Tc1 Cs2 106.90(14) . . ?
O4 Cs1 O4 148.9(7) . 13_544 ?
O4 Cs1 O5 125.9(5) . 13_544 ?
O4 Cs1 O5 70.0(5) 13_544 13_544 ?
O4 Cs1 O5 70.0(5) . . ?
O4 Cs1 O5 125.9(5) 13_544 . ?
O5 Cs1 O5 125.5(7) 13_544 . ?
O4 Cs1 O1 71.0(4) . . ?
O4 Cs1 O1 137.9(5) 13_544 . ?
O5 Cs1 O1 71.8(5) 13_544 . ?
O5 Cs1 O1 66.5(4) . . ?
O4 Cs1 O1 137.9(5) . 13_544 ?
O4 Cs1 O1 71.0(4) 13_544 13_544 ?
O5 Cs1 O1 66.5(4) 13_544 13_544 ?
O5 Cs1 O1 71.8(5) . 13_544 ?
O1 Cs1 O1 77.9(6) . 13_544 ?
O4 Cs1 N1 154.0(5) . 13_544 ?
O4 Cs1 N1 56.8(4) 13_544 13_544 ?
O5 Cs1 N1 53.4(4) 13_544 13_544 ?
O5 Cs1 N1 89.8(5) . 13_544 ?
O1 Cs1 N1 86.1(4) . 13_544 ?
O1 Cs1 N1 18.1(4) 13_544 13_544 ?
O4 Cs1 N1 56.8(4) . . ?
O4 Cs1 N1 154.0(5) 13_544 . ?
O5 Cs1 N1 89.8(5) 13_544 . ?
O5 Cs1 N1 53.4(4) . . ?
O1 Cs1 N1 18.1(4) . . ?
O1 Cs1 N1 86.1(4) 13_544 . ?
N1 Cs1 N1 98.2(6) 13_544 . ?
O4 Cs1 C1 149.8(5) . 13_544 ?
O4 Cs1 C1 15.6(5) 13_544 13_544 ?
O5 Cs1 C1 55.6(5) 13_544 13_544 ?
O5 Cs1 C1 137.3(5) . 13_544 ?
O1 Cs1 C1 126.3(5) . 13_544 ?
O1 Cs1 C1 72.3(5) 13_544 13_544 ?
N1 Cs1 C1 55.4(5) 13_544 13_544 ?
N1 Cs1 C1 144.1(5) . 13_544 ?
O4 Cs1 C1 15.6(5) . . ?
O4 Cs1 C1 149.8(5) 13_544 . ?
O5 Cs1 C1 137.3(5) 13_544 . ?
O5 Cs1 C1 55.6(5) . . ?
O1 Cs1 C1 72.3(5) . . ?
O1 Cs1 C1 126.3(5) 13_544 . ?
N1 Cs1 C1 144.1(5) 13_544 . ?
N1 Cs1 C1 55.4(5) . . ?
C1 Cs1 C1 158.7(7) 13_544 . ?
F1 Cs2 F1 107.4(4) 8_665 . ?
F1 Cs2 O3 53.7(3) 8_665 8_665 ?
F1 Cs2 O3 106.9(4) . 8_665 ?
F1 Cs2 O3 106.9(4) 8_665 . ?
F1 Cs2 O3 53.7(3) . . ?
O3 Cs2 O3 150.4(5) 8_665 . ?
F1 Cs2 F4 83.3(4) 8_665 . ?
F1 Cs2 F4 100.5(4) . . ?
O3 Cs2 F4 134.0(4) 8_665 . ?
O3 Cs2 F4 48.2(4) . . ?
F1 Cs2 F4 100.5(4) 8_665 8_665 ?
F1 Cs2 F4 83.3(4) . 8_665 ?
O3 Cs2 F4 48.2(4) 8_665 8_665 ?
O3 Cs2 F4 134.0(4) . 8_665 ?
F4 Cs2 F4 173.7(8) . 8_665 ?
F1 Cs2 O2 153.1(3) 8_665 . ?
F1 Cs2 O2 51.1(3) . . ?
O3 Cs2 O2 140.3(4) 8_665 . ?
O3 Cs2 O2 49.0(4) . . ?
F4 Cs2 O2 85.5(4) . . ?
F4 Cs2 O2 93.1(4) 8_665 . ?
F1 Cs2 O2 51.1(3) 8_665 8_665 ?
F1 Cs2 O2 153.1(3) . 8_665 ?
O3 Cs2 O2 49.0(4) 8_665 8_665 ?
O3 Cs2 O2 140.3(4) . 8_665 ?
F4 Cs2 O2 93.1(4) . 8_665 ?
F4 Cs2 O2 85.5(4) 8_665 8_665 ?
O2 Cs2 O2 154.3(5) . 8_665 ?
F1 Cs2 F6 100.7(5) 8_665 8_665 ?
F1 Cs2 F6 147.4(5) . 8_665 ?
O3 Cs2 F6 76.8(5) 8_665 8_665 ?
O3 Cs2 F6 132.2(5) . 8_665 ?
F4 Cs2 F6 99.0(6) . 8_665 ?
F4 Cs2 F6 75.5(6) 8_665 8_665 ?
O2 Cs2 F6 105.1(5) . 8_665 ?
O2 Cs2 F6 49.7(5) 8_665 8_665 ?
F1 Cs2 F6 147.4(5) 8_665 . ?
F1 Cs2 F6 100.7(5) . . ?
O3 Cs2 F6 132.2(5) 8_665 . ?
O3 Cs2 F6 76.8(5) . . ?
F4 Cs2 F6 75.5(6) . . ?
F4 Cs2 F6 99.0(6) 8_665 . ?
O2 Cs2 F6 49.7(5) . . ?
O2 Cs2 F6 105.1(5) 8_665 . ?
F6 Cs2 F6 59.6(7) 8_665 . ?
F1 Cs2 Tc1 27.1(2) 8_665 8_665 ?
F1 Cs2 Tc1 121.7(2) . 8_665 ?
O3 Cs2 Tc1 31.8(2) 8_665 8_665 ?
O3 Cs2 Tc1 133.9(3) . 8_665 ?
F4 Cs2 Tc1 102.2(3) . 8_665 ?
F4 Cs2 Tc1 79.8(3) 8_665 8_665 ?
O2 Cs2 Tc1 170.8(3) . 8_665 ?
O2 Cs2 Tc1 31.8(2) 8_665 8_665 ?
F6 Cs2 Tc1 78.8(4) 8_665 8_665 ?
F6 Cs2 Tc1 136.8(4) . 8_665 ?
F1 Cs2 Tc1 121.7(2) 8_665 . ?
F1 Cs2 Tc1 27.1(2) . . ?
O3 Cs2 Tc1 133.9(3) 8_665 . ?
O3 Cs2 Tc1 31.8(2) . . ?
F4 Cs2 Tc1 79.8(3) . . ?
F4 Cs2 Tc1 102.2(3) 8_665 . ?
O2 Cs2 Tc1 31.8(2) . . ?
O2 Cs2 Tc1 170.8(3) 8_665 . ?
F6 Cs2 Tc1 136.8(4) 8_665 . ?
F6 Cs2 Tc1 78.8(4) . . ?
Tc1 Cs2 Tc1 144.15(8) 8_665 . ?

_refine_diff_density_max         1.612
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.145

