#------------------------------------------------------------------------------
#$Date: 2017-09-14 05:40:59 +0300 (Thu, 14 Sep 2017) $
#$Revision: 200871 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044203.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7044203
loop_
_publ_author_name
'Balasekaran, Samundeeswari Mariappan'
'Hagenbach, Adelheid'
'Drees, Markus'
'Abram, Ulrich'
_publ_section_title
;
 [TcII(NO)(trifluoroacetate)4F]2- - Synthesis and Reactions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03084C
_journal_year                    2017
_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
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-24 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7160(10)
_cell_length_b                   9.6050(10)
_cell_length_c                   28.907(2)
_cell_measurement_reflns_used    6422
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.33
_cell_volume                     3736.4(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    Ortep
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.1519
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15306
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0263P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3098
_reflns_number_total             6539
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt03084c1.cif
_cod_data_source_block           tcnotfa4
_cod_database_code               7044203
_shelx_shelxl_version_number     2014/7
_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'
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_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 . .
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
C11 H11B O9 0.97 2.38 3.33(2) 165.4
C21 H21A O9 0.97 2.67 3.577(19) 156.2
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_4
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) . .
