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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_MS_150K
_database_code_depnum_ccdc_archive 'CCDC 1564437'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2793(5)
_cell_length_b                   12.9527(7)
_cell_length_c                   16.6542(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.379(6)
_cell_angle_gamma                90
_cell_volume                     1974.94(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2797
_cell_measurement_theta_min      3.9320
_cell_measurement_theta_max      29.2110

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.105
_shelx_estimated_absorpt_T_min   0.636
_shelx_estimated_absorpt_T_max   0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55693
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8451
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.381
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4028
_reflns_number_gt                3245
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0243P)²+0.5957P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4028
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0668
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.2535(3) 0.4360(2) 0.4070(2) 0.0229(7) Uani 1 1 d . . . . .
H1A H 0.1883 0.3780 0.3866 0.027 Uiso 1 1 calc R U . . .
H1B H 0.2540 0.4426 0.4663 0.027 Uiso 1 1 calc R U . . .
C2 C 0.4065(3) 0.4141(2) 0.39132(18) 0.0228(7) Uani 1 1 d . . . . .
H2A H 0.4745 0.4689 0.4152 0.027 Uiso 1 1 calc R U . . .
H2B H 0.4417 0.3470 0.4155 0.027 Uiso 1 1 calc R U . . .
C3 C 0.5391(3) 0.4144(2) 0.27101(19) 0.0216(7) Uani 1 1 d . . . . .
H3A H 0.5906 0.3475 0.2811 0.026 Uiso 1 1 calc R U . . .
H3B H 0.6022 0.4695 0.2989 0.026 Uiso 1 1 calc R U . . .
C4 C 0.5043(3) 0.4357(2) 0.18125(19) 0.0211(7) Uani 1 1 d . . . . .
H4A H 0.4506 0.3763 0.1533 0.025 Uiso 1 1 calc R U . . .
H4B H 0.5963 0.4443 0.1590 0.025 Uiso 1 1 calc R U . . .
C5 C 0.0357(3) 0.5392(3) 0.3556(2) 0.0240(7) Uani 1 1 d . . . . .
H5A H 0.0034 0.6070 0.3317 0.029 Uiso 1 1 calc R U . . .
H5B H 0.0066 0.5353 0.4101 0.029 Uiso 1 1 calc R U . . .
C6 C -0.0426(4) 0.4551(3) 0.3027(2) 0.0344(9) Uani 1 1 d . . . . .
H6A H 0.0019 0.4473 0.2536 0.052 Uiso 1 1 calc R U . . .
H6B H -0.1458 0.4736 0.2873 0.052 Uiso 1 1 calc R U . . .
H6C H -0.0347 0.3899 0.3330 0.052 Uiso 1 1 calc R U . . .
C7 C 0.2634(3) 0.6265(2) 0.41172(19) 0.0201(7) Uani 1 1 d . . . . .
H7A H 0.2335 0.6888 0.3787 0.024 Uiso 1 1 calc R U . . .
H7B H 0.3711 0.6213 0.4176 0.024 Uiso 1 1 calc R U . . .
C8 C 0.2232(4) 0.6424(3) 0.4958(2) 0.0283(8) Uani 1 1 d . . . . .
H8A H 0.1186 0.6577 0.4906 0.043 Uiso 1 1 calc R U . . .
H8B H 0.2796 0.7002 0.5229 0.043 Uiso 1 1 calc R U . . .
H8C H 0.2454 0.5795 0.5282 0.043 Uiso 1 1 calc R U . . .
C9 C 0.3319(3) 0.5325(2) 0.08090(19) 0.0215(7) Uani 1 1 d . . . . .
H9A H 0.4026 0.5250 0.0427 0.026 Uiso 1 1 calc R U . . .
H9B H 0.2834 0.6003 0.0704 0.026 Uiso 1 1 calc R U . . .
C10 C 0.2174(3) 0.4483(2) 0.0631(2) 0.0268(8) Uani 1 1 d . . . . .
H10A H 0.1590 0.4599 0.0093 0.040 Uiso 1 1 calc R U . . .
H10B H 0.1536 0.4496 0.1045 0.040 Uiso 1 1 calc R U . . .
H10C H 0.2656 0.3809 0.0639 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5075(3) 0.6265(2) 0.18093(19) 0.0198(7) Uani 1 1 d . . . . .
H11A H 0.5625 0.6223 0.2370 0.024 Uiso 1 1 calc R U . . .
H11B H 0.4429 0.6876 0.1784 0.024 Uiso 1 1 calc R U . . .
C12 C 0.6164(4) 0.6439(3) 0.1228(2) 0.0318(8) Uani 1 1 d . . . . .
H12A H 0.5634 0.6550 0.0676 0.048 Uiso 1 1 calc R U . . .
H12B H 0.6796 0.5832 0.1233 0.048 Uiso 1 1 calc R U . . .
H12C H 0.6762 0.7048 0.1402 0.048 Uiso 1 1 calc R U . . .
O1A O 0.1875(2) 0.67520(15) 0.21991(13) 0.0221(5) Uani 1 1 d . . . . .
N2 N 0.1980(3) 0.53362(18) 0.36521(15) 0.0163(5) Uani 1 1 d . . . . .
N3 N 0.3975(3) 0.41131(18) 0.30146(15) 0.0165(5) Uani 1 1 d . . . . .
H3 H 0.3429 0.3479 0.2799 0.020 Uiso 1 1 calc R U . . .
N4 N 0.4133(3) 0.53175(17) 0.16528(15) 0.0160(5) Uani 1 1 d . . . . .
N1A N 0.0607(3) 0.6769(2) 0.17106(18) 0.0285(7) Uani 1 1 d . . . . .
O2A O 0.0105(3) 0.59355(18) 0.15015(16) 0.0386(6) Uani 1 1 d . . . . .
Pd1 Pd 0.28380(2) 0.53625(2) 0.25688(2) 0.01432(8) Uani 1 1 d . . . . .
C13 C 0.6048(3) 0.8006(2) 0.4015(2) 0.0221(7) Uani 1 1 d . . . . .
F1 F 0.65056(19) 0.89767(13) 0.39813(12) 0.0299(5) Uani 1 1 d . . . . .
F2 F 0.5565(2) 0.78924(14) 0.47259(12) 0.0326(5) Uani 1 1 d . . . . .
F3 F 0.49022(18) 0.78832(13) 0.34265(12) 0.0291(4) Uani 1 1 d . . . . .
O3 O 0.7872(2) 0.73459(17) 0.31393(14) 0.0294(5) Uani 1 1 d . . . . .
O4 O 0.6770(2) 0.61090(16) 0.39474(14) 0.0270(5) Uani 1 1 d . . . . .
O5 O 0.8576(2) 0.73208(17) 0.46130(15) 0.0318(6) Uani 1 1 d . . . . .
S1 S 0.74933(8) 0.70926(6) 0.39172(5) 0.02076(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.495(4) . ?
C1 C2 1.512(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.486(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.484(3) . ?
C3 C4 1.502(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.504(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.490(4) . ?
C5 C6 1.510(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.504(4) . ?
C7 C8 1.521(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.483(4) . ?
C9 C10 1.518(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.505(4) . ?
C11 C12 1.525(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O1A N1A 1.317(3) . ?
O1A Pd1 2.059(2) . ?
N2 Pd1 2.088(2) . ?
N3 Pd1 2.007(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.091(2) . ?
N1A O2A 1.205(3) . ?
C13 F1 1.331(3) . ?
C13 F3 1.332(4) . ?
C13 F2 1.340(3) . ?
C13 S1 1.816(3) . ?
O3 S1 1.435(2) . ?
O4 S1 1.445(2) . ?
O5 S1 1.435(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
N2 C1 C2 109.9(2) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.2(3) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.7(2) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C3 C4 N4 110.6(2) . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 114.2(2) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.3(2) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 114.4(2) . . ?
N4 C9 H9A 108.7 . . ?
C10 C9 H9A 108.7 . . ?
N4 C9 H9B 108.7 . . ?
C10 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 115.9(2) . . ?
N4 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N4 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1A O1A Pd1 120.00(18) . . ?
C5 N2 C1 110.9(2) . . ?
C5 N2 C7 109.4(2) . . ?
C1 N2 C7 110.9(2) . . ?
C5 N2 Pd1 115.29(19) . . ?
C1 N2 Pd1 105.41(17) . . ?
C7 N2 Pd1 104.68(16) . . ?
C3 N3 C2 115.8(2) . . ?
C3 N3 Pd1 107.06(17) . . ?
C2 N3 Pd1 107.05(18) . . ?
C3 N3 H3 108.9 . . ?
C2 N3 H3 108.9 . . ?
Pd1 N3 H3 108.9 . . ?
C9 N4 C4 111.0(2) . . ?
C9 N4 C11 110.5(2) . . ?
C4 N4 C11 110.5(2) . . ?
C9 N4 Pd1 115.26(17) . . ?
C4 N4 Pd1 105.50(16) . . ?
C11 N4 Pd1 103.75(17) . . ?
O2A N1A O1A 115.3(3) . . ?
N3 Pd1 O1A 172.77(9) . . ?
N3 Pd1 N2 85.34(9) . . ?
O1A Pd1 N2 93.70(9) . . ?
N3 Pd1 N4 85.26(9) . . ?
O1A Pd1 N4 94.55(9) . . ?
N2 Pd1 N4 167.30(9) . . ?
F1 C13 F3 107.7(2) . . ?
F1 C13 F2 107.2(3) . . ?
F3 C13 F2 107.2(2) . . ?
F1 C13 S1 111.5(2) . . ?
F3 C13 S1 111.6(2) . . ?
F2 C13 S1 111.4(2) . . ?
O3 S1 O5 116.08(14) . . ?
O3 S1 O4 114.63(14) . . ?
O5 S1 O4 114.93(14) . . ?
O3 S1 C13 103.02(14) . . ?
O5 S1 C13 102.93(14) . . ?
O4 S1 C13 102.55(13) . . ?

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
N2 C1 C2 N3 -56.2(3) . . . . ?
N3 C3 C4 N4 54.5(3) . . . . ?
C6 C5 N2 C1 -62.9(3) . . . . ?
C6 C5 N2 C7 174.4(3) . . . . ?
C6 C5 N2 Pd1 56.8(3) . . . . ?
C2 C1 N2 C5 160.9(3) . . . . ?
C2 C1 N2 C7 -77.3(3) . . . . ?
C2 C1 N2 Pd1 35.5(3) . . . . ?
C8 C7 N2 C5 57.8(3) . . . . ?
C8 C7 N2 C1 -64.9(3) . . . . ?
C8 C7 N2 Pd1 -178.1(2) . . . . ?
C4 C3 N3 C2 -167.1(2) . . . . ?
C4 C3 N3 Pd1 -47.8(3) . . . . ?
C1 C2 N3 C3 166.8(2) . . . . ?
C1 C2 N3 Pd1 47.4(3) . . . . ?
C10 C9 N4 C4 65.5(3) . . . . ?
C10 C9 N4 C11 -171.5(2) . . . . ?
C10 C9 N4 Pd1 -54.3(3) . . . . ?
C3 C4 N4 C9 -158.2(2) . . . . ?
C3 C4 N4 C11 78.8(3) . . . . ?
C3 C4 N4 Pd1 -32.7(3) . . . . ?
C12 C11 N4 C9 -56.3(3) . . . . ?
C12 C11 N4 C4 67.0(3) . . . . ?
C12 C11 N4 Pd1 179.6(2) . . . . ?
Pd1 O1A N1A O2A -1.1(4) . . . . ?
F1 C13 S1 O3 -59.3(3) . . . . ?
F3 C13 S1 O3 61.2(2) . . . . ?
F2 C13 S1 O3 -179.0(2) . . . . ?
F1 C13 S1 O5 61.8(2) . . . . ?
F3 C13 S1 O5 -177.7(2) . . . . ?
F2 C13 S1 O5 -57.9(2) . . . . ?
F1 C13 S1 O4 -178.6(2) . . . . ?
F3 C13 S1 O4 -58.1(2) . . . . ?
F2 C13 S1 O4 61.7(2) . . . . ?

_refine_diff_density_max         0.690
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.096

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_VT_150K
_database_code_depnum_ccdc_archive 'CCDC 1564441'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2792(4)
_cell_length_b                   13.0556(5)
_cell_length_c                   16.7552(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.611(4)
_cell_angle_gamma                90
_cell_volume                     2006.94(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3435
_cell_measurement_theta_min      3.9750
_cell_measurement_theta_max      29.0000

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.087
_shelx_estimated_absorpt_T_min   0.640
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8900
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.354
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4090
_reflns_number_gt                3357
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0289P)²+1.2216P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4090
_refine_ls_number_parameters     270
_refine_ls_number_restraints     243
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.040
_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 0.2580(4) 0.4376(3) 0.4084(2) 0.0290(7) Uani 1 1 d . U . . .
H1A H 0.1939 0.3801 0.3871 0.035 Uiso 1 1 calc R U . . .
H1B H 0.2555 0.4431 0.4671 0.035 Uiso 1 1 calc R U . . .
C2 C 0.4116(4) 0.4162(3) 0.39415(19) 0.0297(7) Uani 1 1 d . U . . .
H2A H 0.4787 0.4700 0.4192 0.036 Uiso 1 1 calc R U . . .
H2B H 0.4451 0.3490 0.4173 0.036 Uiso 1 1 calc R U . . .
C3 C 0.5498(4) 0.4182(3) 0.2755(2) 0.0291(7) Uani 1 1 d . U . . .
H3A H 0.6010 0.3519 0.2858 0.035 Uiso 1 1 calc R U . . .
H3B H 0.6124 0.4732 0.3027 0.035 Uiso 1 1 calc R U . . .
C4 C 0.5153(4) 0.4386(3) 0.18564(19) 0.0269(7) Uani 1 1 d . U . . .
H4A H 0.6071 0.4468 0.1629 0.032 Uiso 1 1 calc R U . . .
H4B H 0.4617 0.3795 0.1586 0.032 Uiso 1 1 calc R U . . .
C5 C 0.0403(3) 0.5404(3) 0.3570(2) 0.0298(7) Uani 1 1 d . U . . .
H5A H 0.0086 0.6095 0.3374 0.036 Uiso 1 1 calc R U . . .
H5B H 0.0084 0.5305 0.4103 0.036 Uiso 1 1 calc R U . . .
C6 C -0.0343(4) 0.4619(3) 0.2992(3) 0.0481(10) Uani 1 1 d . U . . .
H6A H 0.0087 0.4631 0.2492 0.072 Uiso 1 1 calc R U . . .
H6B H -0.1384 0.4779 0.2869 0.072 Uiso 1 1 calc R U . . .
H6C H -0.0216 0.3937 0.3237 0.072 Uiso 1 1 calc R U . . .
C7 C 0.2669(4) 0.6261(3) 0.4151(2) 0.0283(7) Uani 1 1 d . U . . .
H7A H 0.2402 0.6886 0.3829 0.034 Uiso 1 1 calc R U . . .
H7B H 0.3744 0.6199 0.4223 0.034 Uiso 1 1 calc R U . . .
C8 C 0.2210(4) 0.6405(3) 0.4982(2) 0.0363(9) Uani 1 1 d . U . . .
H8A H 0.1161 0.6544 0.4919 0.054 Uiso 1 1 calc R U . . .
H8B H 0.2744 0.6984 0.5257 0.054 Uiso 1 1 calc R U . . .
H8C H 0.2429 0.5782 0.5303 0.054 Uiso 1 1 calc R U . . .
C9 C 0.3436(4) 0.5332(3) 0.08583(19) 0.0272(7) Uani 1 1 d . U . . .
H9A H 0.4140 0.5220 0.0477 0.033 Uiso 1 1 calc R U . . .
H9B H 0.2986 0.6014 0.0740 0.033 Uiso 1 1 calc R U . . .
C10 C 0.2262(4) 0.4525(3) 0.0713(2) 0.0354(8) Uani 1 1 d . U . . .
H10A H 0.1725 0.4601 0.0166 0.053 Uiso 1 1 calc R U . . .
H10B H 0.1589 0.4605 0.1107 0.053 Uiso 1 1 calc R U . . .
H10C H 0.2709 0.3843 0.0770 0.053 Uiso 1 1 calc R U . . .
C11 C 0.5184(4) 0.6283(3) 0.1836(2) 0.0286(7) Uani 1 1 d . U . . .
H11A H 0.5729 0.6256 0.2391 0.034 Uiso 1 1 calc R U . . .
H11B H 0.4535 0.6888 0.1806 0.034 Uiso 1 1 calc R U . . .
C12 C 0.6273(4) 0.6448(3) 0.1254(2) 0.0402(9) Uani 1 1 d . U . . .
H12A H 0.5748 0.6571 0.0710 0.060 Uiso 1 1 calc R U . . .
H12B H 0.6886 0.5837 0.1248 0.060 Uiso 1 1 calc R U . . .
H12C H 0.6887 0.7041 0.1428 0.060 Uiso 1 1 calc R U . . .
N2 N 0.2028(3) 0.5355(2) 0.36743(15) 0.0218(5) Uani 1 1 d . U . . .
N3 N 0.4067(3) 0.4158(2) 0.30530(15) 0.0239(6) Uani 1 1 d . U . . .
H3 H 0.3530 0.3531 0.2832 0.029 Uiso 1 1 calc R U . . .
N4 N 0.4247(3) 0.53375(19) 0.17015(15) 0.0229(5) Uani 1 1 d . U . . .
Pd1 Pd 0.29310(3) 0.53876(2) 0.26064(2) 0.01989(9) Uani 1 1 d . U . . .
N1_a N 0.1858(17) 0.6657(10) 0.2182(10) 0.027(2) Uani 0.443(7) 1 d D U P A 1
O1_a O 0.2330(7) 0.7454(5) 0.2478(4) 0.051(2) Uani 0.443(7) 1 d D U P A 1
O2_a O 0.0772(14) 0.6596(7) 0.1678(8) 0.051(2) Uani 0.443(7) 1 d D U P A 1
N1A_b N 0.0682(10) 0.6811(5) 0.1735(6) 0.0315(18) Uani 0.557(7) 1 d D U P A 2
O1A_b O 0.1918(10) 0.6751(7) 0.2219(6) 0.0252(17) Uani 0.557(7) 1 d D U P A 2
O2A_b O 0.0169(5) 0.5932(4) 0.1528(3) 0.0406(16) Uani 0.557(7) 1 d D U P A 2
C13 C 0.6085(4) 0.8045(3) 0.4054(2) 0.0260(6) Uani 1 1 d . U . . .
F1 F 0.6552(2) 0.90120(14) 0.40167(12) 0.0364(5) Uani 1 1 d . U . . .
F2 F 0.5586(2) 0.79388(16) 0.47530(12) 0.0393(5) Uani 1 1 d . U . . .
F3 F 0.4953(2) 0.79353(16) 0.34634(12) 0.0366(5) Uani 1 1 d . U . . .
O3 O 0.7913(3) 0.73782(18) 0.31733(14) 0.0357(6) Uani 1 1 d . U . . .
O4 O 0.6784(3) 0.61603(18) 0.39757(14) 0.0330(6) Uani 1 1 d . U . . .
O5 O 0.8593(3) 0.7345(2) 0.46326(16) 0.0404(6) Uani 1 1 d . U . . .
S1 S 0.75175(9) 0.71320(6) 0.39467(5) 0.02592(19) Uani 1 1 d . 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
C1 N2 1.505(4) . ?
C1 C2 1.506(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.483(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.488(4) . ?
C3 C4 1.515(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.501(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.493(4) . ?
C5 C6 1.505(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.499(4) . ?
C7 C8 1.527(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.498(4) . ?
C9 C10 1.510(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.508(4) . ?
C11 C12 1.521(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pd1 2.087(2) . ?
N3 Pd1 2.003(3) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.086(3) . ?
Pd1 N1_a 2.008(17) . ?
Pd1 O1A_b 2.071(10) . ?
N1_a O1_a 1.206(9) . ?
N1_a O2_a 1.217(9) . ?
N1A_b O2A_b 1.271(8) . ?
N1A_b O1A_b 1.304(7) . ?
C13 F2 1.330(4) . ?
C13 F3 1.338(4) . ?
C13 F1 1.339(4) . ?
C13 S1 1.814(3) . ?
O3 S1 1.435(2) . ?
O4 S1 1.444(2) . ?
O5 S1 1.432(3) . ?

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
N2 C1 C2 110.5(3) . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.8(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.7(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.3(3) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 113.9(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.1(3) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.8(3) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.3(3) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C7 110.0(2) . . ?
C5 N2 C1 111.0(3) . . ?
C7 N2 C1 110.2(3) . . ?
C5 N2 Pd1 115.3(2) . . ?
C7 N2 Pd1 105.25(19) . . ?
C1 N2 Pd1 104.80(18) . . ?
C2 N3 C3 116.3(3) . . ?
C2 N3 Pd1 107.9(2) . . ?
C3 N3 Pd1 107.71(19) . . ?
C2 N3 H3 108.2 . . ?
C3 N3 H3 108.2 . . ?
Pd1 N3 H3 108.2 . . ?
C9 N4 C4 110.4(2) . . ?
C9 N4 C11 110.0(2) . . ?
C4 N4 C11 110.9(3) . . ?
C9 N4 Pd1 114.80(19) . . ?
C4 N4 Pd1 105.90(18) . . ?
C11 N4 Pd1 104.65(18) . . ?
N3 Pd1 N1_a 177.6(3) . . ?
N3 Pd1 O1A_b 174.0(2) . . ?
N3 Pd1 N4 85.05(10) . . ?
N1_a Pd1 N4 94.7(5) . . ?
O1A_b Pd1 N4 95.0(3) . . ?
N3 Pd1 N2 85.40(10) . . ?
N1_a Pd1 N2 94.5(5) . . ?
O1A_b Pd1 N2 93.7(3) . . ?
N4 Pd1 N2 167.63(10) . . ?
O1_a N1_a O2_a 123.6(15) . . ?
O1_a N1_a Pd1 115.8(11) . . ?
O2_a N1_a Pd1 120.5(9) . . ?
O2A_b N1A_b O1A_b 112.0(6) . . ?
N1A_b O1A_b Pd1 124.2(5) . . ?
F2 C13 F3 107.6(3) . . ?
F2 C13 F1 107.3(3) . . ?
F3 C13 F1 106.8(3) . . ?
F2 C13 S1 112.1(2) . . ?
F3 C13 S1 111.2(2) . . ?
F1 C13 S1 111.6(2) . . ?
O5 S1 O3 116.07(16) . . ?
O5 S1 O4 114.78(15) . . ?
O3 S1 O4 114.37(15) . . ?
O5 S1 C13 103.05(15) . . ?
O3 S1 C13 103.44(15) . . ?
O4 S1 C13 102.57(15) . . ?

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
N2 C1 C2 N3 -55.7(4) . . . . ?
N3 C3 C4 N4 54.6(4) . . . . ?
C6 C5 N2 C7 171.0(3) . . . . ?
C6 C5 N2 C1 -66.7(4) . . . . ?
C6 C5 N2 Pd1 52.2(4) . . . . ?
C8 C7 N2 C5 56.6(4) . . . . ?
C8 C7 N2 C1 -66.1(4) . . . . ?
C8 C7 N2 Pd1 -178.6(2) . . . . ?
C2 C1 N2 C5 161.0(3) . . . . ?
C2 C1 N2 C7 -76.8(3) . . . . ?
C2 C1 N2 Pd1 36.0(3) . . . . ?
C1 C2 N3 C3 167.5(3) . . . . ?
C1 C2 N3 Pd1 46.4(3) . . . . ?
C4 C3 N3 C2 -169.0(3) . . . . ?
C4 C3 N3 Pd1 -47.8(3) . . . . ?
C10 C9 N4 C4 68.1(3) . . . . ?
C10 C9 N4 C11 -169.2(3) . . . . ?
C10 C9 N4 Pd1 -51.5(3) . . . . ?
C3 C4 N4 C9 -158.3(3) . . . . ?
C3 C4 N4 C11 79.5(3) . . . . ?
C3 C4 N4 Pd1 -33.5(3) . . . . ?
C12 C11 N4 C9 -56.3(4) . . . . ?
C12 C11 N4 C4 66.1(4) . . . . ?
C12 C11 N4 Pd1 179.9(3) . . . . ?
O2A_b N1A_b O1A_b Pd1 -0.1(11) . . . . ?
F2 C13 S1 O5 -58.0(3) . . . . ?
F3 C13 S1 O5 -178.4(2) . . . . ?
F1 C13 S1 O5 62.4(3) . . . . ?
F2 C13 S1 O3 -179.3(2) . . . . ?
F3 C13 S1 O3 60.3(3) . . . . ?
F1 C13 S1 O3 -58.9(3) . . . . ?
F2 C13 S1 O4 61.5(3) . . . . ?
F3 C13 S1 O4 -58.9(3) . . . . ?
F1 C13 S1 O4 -178.1(2) . . . . ?

_refine_diff_density_max         0.579
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.091

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_GS_150K
_database_code_depnum_ccdc_archive 'CCDC 1564438'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2318(4)
_cell_length_b                   13.1472(6)
_cell_length_c                   17.0207(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.736(5)
_cell_angle_gamma                90
_cell_volume                     2051.58(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3384
_cell_measurement_theta_min      3.8890
_cell_measurement_theta_max      29.4440

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.064
_shelx_estimated_absorpt_T_min   0.646
_shelx_estimated_absorpt_T_max   0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9030
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.325
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4196
_reflns_number_gt                3410
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0255P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4196
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0596
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.2570(3) 0.4378(2) 0.40799(18) 0.0255(7) Uani 1 1 d . . . . .
H1A H 0.1942 0.3825 0.3836 0.031 Uiso 1 1 calc R U . . .
H1B H 0.2465 0.4397 0.4652 0.031 Uiso 1 1 calc R U . . .
C2 C 0.4141(3) 0.4168(2) 0.39670(17) 0.0235(7) Uani 1 1 d . . . . .
H2A H 0.4793 0.4685 0.4243 0.028 Uiso 1 1 calc R U . . .
H2B H 0.4442 0.3487 0.4175 0.028 Uiso 1 1 calc R U . . .
C3 C 0.5643(3) 0.4241(2) 0.28138(18) 0.0233(7) Uani 1 1 d . . . . .
H3A H 0.6149 0.3582 0.2914 0.028 Uiso 1 1 calc R U . . .
H3B H 0.6254 0.4784 0.3085 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5368(3) 0.4448(2) 0.19445(18) 0.0249(7) Uani 1 1 d . . . . .
H4A H 0.4849 0.3862 0.1675 0.030 Uiso 1 1 calc R U . . .
H4B H 0.6310 0.4530 0.1727 0.030 Uiso 1 1 calc R U . . .
C5 C 0.0466(3) 0.5437(2) 0.35825(19) 0.0306(7) Uani 1 1 d . . . . .
H5A H 0.0178 0.6147 0.3448 0.037 Uiso 1 1 calc R U . . .
H5B H 0.0081 0.5263 0.4084 0.037 Uiso 1 1 calc R U . . .
C6 C -0.0225(3) 0.4744(3) 0.2939(2) 0.0425(9) Uani 1 1 d . . . . .
H6A H 0.0223 0.4862 0.2453 0.064 Uiso 1 1 calc R U . . .
H6B H -0.1273 0.4886 0.2842 0.064 Uiso 1 1 calc R U . . .
H6C H -0.0074 0.4034 0.3105 0.064 Uiso 1 1 calc R U . . .
C7 C 0.2701(3) 0.6246(2) 0.42126(17) 0.0249(7) Uani 1 1 d . . . . .
H7A H 0.2467 0.6886 0.3918 0.030 Uiso 1 1 calc R U . . .
H7B H 0.3777 0.6181 0.4293 0.030 Uiso 1 1 calc R U . . .
C8 C 0.2155(3) 0.6337(3) 0.50208(19) 0.0363(8) Uani 1 1 d . . . . .
H8A H 0.1103 0.6469 0.4951 0.054 Uiso 1 1 calc R U . . .
H8B H 0.2661 0.6898 0.5316 0.054 Uiso 1 1 calc R U . . .
H8C H 0.2350 0.5701 0.5315 0.054 Uiso 1 1 calc R U . . .
C9 C 0.3701(3) 0.5376(2) 0.09633(18) 0.0280(7) Uani 1 1 d . . . . .
H9A H 0.4414 0.5198 0.0594 0.034 Uiso 1 1 calc R U . . .
H9B H 0.3324 0.6065 0.0823 0.034 Uiso 1 1 calc R U . . .
C10 C 0.2447(4) 0.4626(2) 0.0854(2) 0.0359(8) Uani 1 1 d . . . . .
H10A H 0.1996 0.4645 0.0304 0.054 Uiso 1 1 calc R U . . .
H10B H 0.1720 0.4809 0.1206 0.054 Uiso 1 1 calc R U . . .
H10C H 0.2813 0.3939 0.0983 0.054 Uiso 1 1 calc R U . . .
C11 C 0.5416(3) 0.6325(2) 0.19113(19) 0.0277(7) Uani 1 1 d . . . . .
H11A H 0.5940 0.6296 0.2453 0.033 Uiso 1 1 calc R U . . .
H11B H 0.4780 0.6934 0.1882 0.033 Uiso 1 1 calc R U . . .
C12 C 0.6538(4) 0.6462(3) 0.1326(2) 0.0472(10) Uani 1 1 d . . . . .
H12A H 0.6032 0.6593 0.0797 0.071 Uiso 1 1 calc R U . . .
H12B H 0.7125 0.5842 0.1315 0.071 Uiso 1 1 calc R U . . .
H12C H 0.7175 0.7038 0.1491 0.071 Uiso 1 1 calc R U . . .
N1 N 0.1996(3) 0.67013(18) 0.22526(15) 0.0242(6) Uani 1 1 d . . . . .
N2 N 0.2096(2) 0.53751(16) 0.37071(14) 0.0187(5) Uani 1 1 d . . . . .
N3 N 0.4192(2) 0.42157(16) 0.31012(14) 0.0164(5) Uani 1 1 d . . . . .
H3 H 0.3666 0.3604 0.2863 0.020 Uiso 1 1 calc R U . . .
N4 N 0.4465(2) 0.53977(16) 0.17850(14) 0.0194(5) Uani 1 1 d . . . . .
O1 O 0.2389(3) 0.75236(17) 0.25489(16) 0.0525(7) Uani 1 1 d . . . . .
O2 O 0.0959(3) 0.66826(18) 0.17400(16) 0.0579(8) Uani 1 1 d . . . . .
Pd1 Pd 0.30898(2) 0.54438(2) 0.26725(2) 0.01533(7) Uani 1 1 d . . . . .
C13 C 0.6102(3) 0.8119(2) 0.41177(19) 0.0270(7) Uani 1 1 d . . . . .
F1 F 0.6607(2) 0.90649(12) 0.41021(12) 0.0385(5) Uani 1 1 d . . . . .
F2 F 0.5560(2) 0.80111(14) 0.48065(11) 0.0439(5) Uani 1 1 d . . . . .
F3 F 0.50045(19) 0.80320(14) 0.35495(12) 0.0439(5) Uani 1 1 d . . . . .
O3 O 0.7956(2) 0.74294(16) 0.32478(14) 0.0368(6) Uani 1 1 d . . . . .
O4 O 0.6751(2) 0.62358(14) 0.40325(13) 0.0314(5) Uani 1 1 d . . . . .
O5 O 0.8577(2) 0.73812(17) 0.46786(15) 0.0428(6) Uani 1 1 d . . . . .
S1 S 0.75190(8) 0.71882(5) 0.40084(5) 0.02488(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.499(3) . ?
C1 C2 1.510(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.481(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.480(3) . ?
C3 C4 1.497(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.508(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.497(3) . ?
C5 C6 1.507(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.500(4) . ?
C7 C8 1.524(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.491(4) . ?
C9 C10 1.516(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.503(3) . ?
C11 C12 1.530(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 O2 1.217(3) . ?
N1 O1 1.230(3) . ?
N1 Pd1 2.024(2) . ?
N2 Pd1 2.081(2) . ?
N3 Pd1 2.000(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.085(2) . ?
C13 F3 1.321(3) . ?
C13 F1 1.330(3) . ?
C13 F2 1.335(3) . ?
C13 S1 1.817(3) . ?
O3 S1 1.436(2) . ?
O4 S1 1.442(2) . ?
O5 S1 1.434(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
N2 C1 C2 110.1(2) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 105.2(2) . . ?
N3 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
N3 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
N3 C3 C4 106.0(2) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 110.8(2) . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 113.7(2) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 115.9(2) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.4(2) . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 115.5(2) . . ?
N4 C11 H11A 108.4 . . ?
C12 C11 H11A 108.4 . . ?
N4 C11 H11B 108.4 . . ?
C12 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 N1 O1 118.8(2) . . ?
O2 N1 Pd1 123.7(2) . . ?
O1 N1 Pd1 117.5(2) . . ?
C5 N2 C1 110.3(2) . . ?
C5 N2 C7 109.9(2) . . ?
C1 N2 C7 110.7(2) . . ?
C5 N2 Pd1 114.42(18) . . ?
C1 N2 Pd1 105.09(15) . . ?
C7 N2 Pd1 106.31(16) . . ?
C3 N3 C2 117.8(2) . . ?
C3 N3 Pd1 107.63(16) . . ?
C2 N3 Pd1 108.85(16) . . ?
C3 N3 H3 107.4 . . ?
C2 N3 H3 107.4 . . ?
Pd1 N3 H3 107.4 . . ?
C9 N4 C11 110.7(2) . . ?
C9 N4 C4 110.1(2) . . ?
C11 N4 C4 110.2(2) . . ?
C9 N4 Pd1 114.78(17) . . ?
C11 N4 Pd1 105.53(16) . . ?
C4 N4 Pd1 105.32(16) . . ?
N3 Pd1 N1 179.02(10) . . ?
N3 Pd1 N2 84.96(9) . . ?
N1 Pd1 N2 94.76(9) . . ?
N3 Pd1 N4 85.06(9) . . ?
N1 Pd1 N4 95.11(9) . . ?
N2 Pd1 N4 168.03(9) . . ?
F3 C13 F1 107.9(2) . . ?
F3 C13 F2 107.4(2) . . ?
F1 C13 F2 106.6(3) . . ?
F3 C13 S1 111.5(2) . . ?
F1 C13 S1 111.69(19) . . ?
F2 C13 S1 111.5(2) . . ?
O5 S1 O3 116.16(14) . . ?
O5 S1 O4 114.97(14) . . ?
O3 S1 O4 114.10(13) . . ?
O5 S1 C13 103.34(14) . . ?
O3 S1 C13 103.02(14) . . ?
O4 S1 C13 102.69(13) . . ?

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
N2 C1 C2 N3 -56.0(3) . . . . ?
N3 C3 C4 N4 54.5(3) . . . . ?
C6 C5 N2 C1 -70.8(3) . . . . ?
C6 C5 N2 C7 166.9(3) . . . . ?
C6 C5 N2 Pd1 47.4(3) . . . . ?
C2 C1 N2 C5 161.8(2) . . . . ?
C2 C1 N2 C7 -76.4(3) . . . . ?
C2 C1 N2 Pd1 38.0(3) . . . . ?
C8 C7 N2 C5 57.2(3) . . . . ?
C8 C7 N2 C1 -64.9(3) . . . . ?
C8 C7 N2 Pd1 -178.5(2) . . . . ?
C4 C3 N3 C2 -171.6(2) . . . . ?
C4 C3 N3 Pd1 -48.2(2) . . . . ?
C1 C2 N3 C3 168.2(2) . . . . ?
C1 C2 N3 Pd1 45.4(2) . . . . ?
C10 C9 N4 C11 -165.1(2) . . . . ?
C10 C9 N4 C4 72.8(3) . . . . ?
C10 C9 N4 Pd1 -45.8(3) . . . . ?
C12 C11 N4 C9 -55.4(3) . . . . ?
C12 C11 N4 C4 66.6(3) . . . . ?
C12 C11 N4 Pd1 179.8(2) . . . . ?
C3 C4 N4 C9 -157.1(2) . . . . ?
C3 C4 N4 C11 80.5(3) . . . . ?
C3 C4 N4 Pd1 -32.9(3) . . . . ?
F3 C13 S1 O5 -178.5(2) . . . . ?
F1 C13 S1 O5 60.7(3) . . . . ?
F2 C13 S1 O5 -58.4(2) . . . . ?
F3 C13 S1 O3 60.1(2) . . . . ?
F1 C13 S1 O3 -60.6(3) . . . . ?
F2 C13 S1 O3 -179.8(2) . . . . ?
F3 C13 S1 O4 -58.7(2) . . . . ?
F1 C13 S1 O4 -179.4(2) . . . . ?
F2 C13 S1 O4 61.5(2) . . . . ?

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
N3 H3 N1 1.00 2.58 3.512(3) 155.6 2_545
N3 H3 O1 1.00 1.82 2.815(3) 176.5 2_545
N3 H3 O2 1.00 2.63 3.345(3) 128.7 2_545

_refine_diff_density_max         0.601
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.088

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_VT_140K
_database_code_depnum_ccdc_archive 'CCDC 1564440'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2754(4)
_cell_length_b                   13.0534(5)
_cell_length_c                   16.7384(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.677(4)
_cell_angle_gamma                90
_cell_volume                     2003.41(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    3531
_cell_measurement_theta_min      3.9750
_cell_measurement_theta_max      29.1580

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.089
_shelx_estimated_absorpt_T_min   0.640
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8896
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.355
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4085
_reflns_number_gt                3343
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0282P)²+1.1611P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4085
_refine_ls_number_parameters     270
_refine_ls_number_restraints     243
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0676
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.056
_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 0.2573(4) 0.4375(2) 0.40827(19) 0.0263(7) Uani 1 1 d . U . . .
H1A H 0.1931 0.3802 0.3866 0.032 Uiso 1 1 calc R U . . .
H1B H 0.2544 0.4428 0.4670 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4112(4) 0.4163(3) 0.39426(18) 0.0270(7) Uani 1 1 d . U . . .
H2A H 0.4781 0.4704 0.4192 0.032 Uiso 1 1 calc R U . . .
H2B H 0.4450 0.3493 0.4177 0.032 Uiso 1 1 calc R U . . .
C3 C 0.5491(4) 0.4179(3) 0.27561(19) 0.0266(7) Uani 1 1 d . U . . .
H3A H 0.6005 0.3517 0.2862 0.032 Uiso 1 1 calc R U . . .
H3B H 0.6114 0.4731 0.3028 0.032 Uiso 1 1 calc R U . . .
C4 C 0.5147(4) 0.4380(3) 0.18528(19) 0.0270(7) Uani 1 1 d . U . . .
H4A H 0.6066 0.4461 0.1626 0.032 Uiso 1 1 calc R U . . .
H4B H 0.4609 0.3790 0.1582 0.032 Uiso 1 1 calc R U . . .
C5 C 0.0406(3) 0.5411(3) 0.35670(19) 0.0268(7) Uani 1 1 d . U . . .
H5A H 0.0097 0.6102 0.3366 0.032 Uiso 1 1 calc R U . . .
H5B H 0.0083 0.5321 0.4100 0.032 Uiso 1 1 calc R U . . .
C6 C -0.0349(4) 0.4620(3) 0.2989(2) 0.0451(10) Uani 1 1 d . U . . .
H6A H 0.0108 0.4605 0.2498 0.068 Uiso 1 1 calc R U . . .
H6B H -0.1382 0.4799 0.2847 0.068 Uiso 1 1 calc R U . . .
H6C H -0.0262 0.3944 0.3246 0.068 Uiso 1 1 calc R U . . .
C7 C 0.2674(4) 0.6264(2) 0.41523(19) 0.0259(7) Uani 1 1 d . U . . .
H7A H 0.2403 0.6889 0.3829 0.031 Uiso 1 1 calc R U . . .
H7B H 0.3750 0.6206 0.4224 0.031 Uiso 1 1 calc R U . . .
C8 C 0.2214(4) 0.6407(3) 0.4982(2) 0.0334(8) Uani 1 1 d . U . . .
H8A H 0.1162 0.6537 0.4919 0.050 Uiso 1 1 calc R U . . .
H8B H 0.2740 0.6989 0.5257 0.050 Uiso 1 1 calc R U . . .
H8C H 0.2443 0.5785 0.5305 0.050 Uiso 1 1 calc R U . . .
C9 C 0.3431(4) 0.5330(2) 0.08530(18) 0.0256(7) Uani 1 1 d . U . . .
H9A H 0.4134 0.5212 0.0472 0.031 Uiso 1 1 calc R U . . .
H9B H 0.2984 0.6012 0.0732 0.031 Uiso 1 1 calc R U . . .
C10 C 0.2253(4) 0.4526(3) 0.0712(2) 0.0330(8) Uani 1 1 d . U . . .
H10A H 0.1700 0.4609 0.0169 0.049 Uiso 1 1 calc R U . . .
H10B H 0.1594 0.4603 0.1114 0.049 Uiso 1 1 calc R U . . .
H10C H 0.2698 0.3844 0.0761 0.049 Uiso 1 1 calc R U . . .
C11 C 0.5185(4) 0.6279(2) 0.18336(19) 0.0262(7) Uani 1 1 d . U . . .
H11A H 0.5731 0.6249 0.2389 0.031 Uiso 1 1 calc R U . . .
H11B H 0.4538 0.6885 0.1805 0.031 Uiso 1 1 calc R U . . .
C12 C 0.6272(4) 0.6444(3) 0.1253(2) 0.0374(9) Uani 1 1 d . U . . .
H12A H 0.5746 0.6577 0.0710 0.056 Uiso 1 1 calc R U . . .
H12B H 0.6876 0.5830 0.1242 0.056 Uiso 1 1 calc R U . . .
H12C H 0.6895 0.7031 0.1432 0.056 Uiso 1 1 calc R U . . .
N2 N 0.2034(3) 0.53532(19) 0.36749(15) 0.0200(5) Uani 1 1 d . U . . .
N3 N 0.4063(3) 0.4155(2) 0.30517(15) 0.0228(6) Uani 1 1 d . U . . .
H3 H 0.3525 0.3527 0.2831 0.027 Uiso 1 1 calc R U . . .
N4 N 0.4241(3) 0.53362(19) 0.16982(15) 0.0212(5) Uani 1 1 d . U . . .
Pd1 Pd 0.29279(3) 0.53869(2) 0.26049(2) 0.01868(8) Uani 1 1 d . U . . .
N1_a N 0.1884(16) 0.6631(9) 0.2190(9) 0.026(2) Uani 0.433(7) 1 d D U P A 1
O1_a O 0.2337(7) 0.7444(5) 0.2475(4) 0.050(2) Uani 0.433(7) 1 d D U P A 1
O2_a O 0.0793(14) 0.6605(7) 0.1676(8) 0.050(2) Uani 0.433(7) 1 d D U P A 1
N1A_b N 0.0657(9) 0.6800(5) 0.1727(6) 0.0275(16) Uani 0.567(7) 1 d D U P A 2
O1A_b O 0.1899(9) 0.6762(6) 0.2214(6) 0.0225(16) Uani 0.567(7) 1 d D U P A 2
O2A_b O 0.0173(5) 0.5928(3) 0.1530(3) 0.0397(15) Uani 0.567(7) 1 d D U P A 2
C13 C 0.6079(3) 0.8045(2) 0.40470(19) 0.0242(6) Uani 1 1 d . U . . .
F1 F 0.6554(2) 0.90105(14) 0.40149(12) 0.0337(5) Uani 1 1 d . U . . .
F2 F 0.5587(2) 0.79377(15) 0.47513(11) 0.0371(5) Uani 1 1 d . U . . .
F3 F 0.4948(2) 0.79341(15) 0.34597(12) 0.0341(5) Uani 1 1 d . U . . .
O3 O 0.7911(3) 0.73808(18) 0.31699(14) 0.0333(6) Uani 1 1 d . U . . .
O4 O 0.6779(3) 0.61584(17) 0.39736(13) 0.0309(5) Uani 1 1 d . U . . .
O5 O 0.8595(3) 0.73458(19) 0.46323(15) 0.0371(6) Uani 1 1 d . U . . .
S1 S 0.75187(9) 0.71309(6) 0.39453(5) 0.02412(18) Uani 1 1 d . 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
C1 N2 1.498(4) . ?
C1 C2 1.507(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.485(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.483(4) . ?
C3 C4 1.520(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.505(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.496(4) . ?
C5 C6 1.513(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.504(4) . ?
C7 C8 1.525(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.499(4) . ?
C9 C10 1.508(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.507(4) . ?
C11 C12 1.517(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pd1 2.084(2) . ?
N3 Pd1 2.004(3) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.086(2) . ?
Pd1 N1_a 1.964(15) . ?
Pd1 O1A_b 2.091(8) . ?
N1_a O1_a 1.213(9) . ?
N1_a O2_a 1.226(8) . ?
N1A_b O2A_b 1.251(7) . ?
N1A_b O1A_b 1.307(6) . ?
C13 F3 1.333(4) . ?
C13 F2 1.334(4) . ?
C13 F1 1.338(4) . ?
C13 S1 1.818(3) . ?
O3 S1 1.437(2) . ?
O4 S1 1.447(2) . ?
O5 S1 1.432(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
N2 C1 C2 110.1(3) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.7(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.8(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.0(3) . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 113.8(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.0(3) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.6(3) . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.5(3) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 111.1(2) . . ?
C5 N2 C7 109.5(2) . . ?
C1 N2 C7 110.7(2) . . ?
C5 N2 Pd1 114.86(19) . . ?
C1 N2 Pd1 105.13(17) . . ?
C7 N2 Pd1 105.28(18) . . ?
C3 N3 C2 116.2(3) . . ?
C3 N3 Pd1 107.66(19) . . ?
C2 N3 Pd1 107.68(19) . . ?
C3 N3 H3 108.4 . . ?
C2 N3 H3 108.4 . . ?
Pd1 N3 H3 108.4 . . ?
C9 N4 C4 110.2(2) . . ?
C9 N4 C11 110.1(2) . . ?
C4 N4 C11 110.8(3) . . ?
C9 N4 Pd1 114.99(19) . . ?
C4 N4 Pd1 105.88(18) . . ?
C11 N4 Pd1 104.73(18) . . ?
N1_a Pd1 N3 177.6(4) . . ?
N1_a Pd1 N2 94.7(5) . . ?
N3 Pd1 N2 85.24(10) . . ?
N1_a Pd1 N4 94.6(5) . . ?
N3 Pd1 N4 85.10(10) . . ?
N2 Pd1 N4 167.49(10) . . ?
N3 Pd1 O1A_b 174.2(2) . . ?
N2 Pd1 O1A_b 93.7(3) . . ?
N4 Pd1 O1A_b 95.1(3) . . ?
O1_a N1_a O2_a 120.1(13) . . ?
O1_a N1_a Pd1 117.5(10) . . ?
O2_a N1_a Pd1 122.4(8) . . ?
O2A_b N1A_b O1A_b 112.2(6) . . ?
N1A_b O1A_b Pd1 123.1(5) . . ?
F3 C13 F2 107.7(3) . . ?
F3 C13 F1 107.5(3) . . ?
F2 C13 F1 107.1(3) . . ?
F3 C13 S1 111.5(2) . . ?
F2 C13 S1 111.6(2) . . ?
F1 C13 S1 111.3(2) . . ?
O5 S1 O3 116.10(16) . . ?
O5 S1 O4 114.95(15) . . ?
O3 S1 O4 114.49(14) . . ?
O5 S1 C13 103.24(15) . . ?
O3 S1 C13 103.01(15) . . ?
O4 S1 C13 102.38(15) . . ?

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
N2 C1 C2 N3 -56.2(3) . . . . ?
N3 C3 C4 N4 54.8(3) . . . . ?
C6 C5 N2 C1 -66.1(4) . . . . ?
C6 C5 N2 C7 171.2(3) . . . . ?
C6 C5 N2 Pd1 53.0(3) . . . . ?
C2 C1 N2 C5 161.3(3) . . . . ?
C2 C1 N2 C7 -76.7(3) . . . . ?
C2 C1 N2 Pd1 36.5(3) . . . . ?
C8 C7 N2 C5 57.2(4) . . . . ?
C8 C7 N2 C1 -65.7(3) . . . . ?
C8 C7 N2 Pd1 -178.8(2) . . . . ?
C4 C3 N3 C2 -168.9(3) . . . . ?
C4 C3 N3 Pd1 -48.2(3) . . . . ?
C1 C2 N3 C3 167.5(3) . . . . ?
C1 C2 N3 Pd1 46.8(3) . . . . ?
C10 C9 N4 C4 68.5(3) . . . . ?
C10 C9 N4 C11 -169.1(3) . . . . ?
C10 C9 N4 Pd1 -51.1(3) . . . . ?
C3 C4 N4 C9 -158.4(3) . . . . ?
C3 C4 N4 C11 79.5(3) . . . . ?
C3 C4 N4 Pd1 -33.5(3) . . . . ?
C12 C11 N4 C9 -56.0(4) . . . . ?
C12 C11 N4 C4 66.1(4) . . . . ?
C12 C11 N4 Pd1 179.9(2) . . . . ?
O2A_b N1A_b O1A_b Pd1 0.0(10) . . . . ?
F3 C13 S1 O5 -178.2(2) . . . . ?
F2 C13 S1 O5 -57.7(3) . . . . ?
F1 C13 S1 O5 61.8(3) . . . . ?
F3 C13 S1 O3 60.6(2) . . . . ?
F2 C13 S1 O3 -179.0(2) . . . . ?
F1 C13 S1 O3 -59.4(2) . . . . ?
F3 C13 S1 O4 -58.5(2) . . . . ?
F2 C13 S1 O4 61.9(2) . . . . ?
F1 C13 S1 O4 -178.5(2) . . . . ?

_refine_diff_density_max         0.666
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.091

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_VT_130K
_database_code_depnum_ccdc_archive 'CCDC 1564439'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2710(4)
_cell_length_b                   13.0533(5)
_cell_length_c                   16.7207(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.733(4)
_cell_angle_gamma                90
_cell_volume                     2000.03(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    3628
_cell_measurement_theta_min      3.8420
_cell_measurement_theta_max      28.5010

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.091
_shelx_estimated_absorpt_T_min   0.640
_shelx_estimated_absorpt_T_max   0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8859
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.356
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4074
_reflns_number_gt                3375
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0247P)²+1.5923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4074
_refine_ls_number_parameters     270
_refine_ls_number_restraints     243
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.044
_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 0.2575(4) 0.4376(2) 0.40828(19) 0.0256(7) Uani 1 1 d . U . . .
H1A H 0.1930 0.3803 0.3868 0.031 Uiso 1 1 calc R U . . .
H1B H 0.2551 0.4430 0.4671 0.031 Uiso 1 1 calc R U . . .
C2 C 0.4111(4) 0.4158(3) 0.39422(18) 0.0268(7) Uani 1 1 d . U . . .
H2A H 0.4786 0.4694 0.4195 0.032 Uiso 1 1 calc R U . . .
H2B H 0.4443 0.3485 0.4175 0.032 Uiso 1 1 calc R U . . .
C3 C 0.5488(4) 0.4173(3) 0.27532(19) 0.0262(7) Uani 1 1 d . U . . .
H3A H 0.5997 0.3508 0.2858 0.031 Uiso 1 1 calc R U . . .
H3B H 0.6118 0.4721 0.3025 0.031 Uiso 1 1 calc R U . . .
C4 C 0.5142(4) 0.4374(2) 0.18521(18) 0.0245(7) Uani 1 1 d . U . . .
H4A H 0.6061 0.4454 0.1625 0.029 Uiso 1 1 calc R U . . .
H4B H 0.4602 0.3784 0.1581 0.029 Uiso 1 1 calc R U . . .
C5 C 0.0403(3) 0.5408(3) 0.35690(19) 0.0263(7) Uani 1 1 d . U . . .
H5A H 0.0090 0.6100 0.3372 0.032 Uiso 1 1 calc R U . . .
H5B H 0.0085 0.5311 0.4103 0.032 Uiso 1 1 calc R U . . .
C6 C -0.0355(4) 0.4622(3) 0.2987(2) 0.0441(10) Uani 1 1 d . U . . .
H6A H 0.0098 0.4613 0.2494 0.066 Uiso 1 1 calc R U . . .
H6B H -0.1390 0.4801 0.2849 0.066 Uiso 1 1 calc R U . . .
H6C H -0.0265 0.3944 0.3241 0.066 Uiso 1 1 calc R U . . .
C7 C 0.2675(4) 0.6264(2) 0.41528(18) 0.0249(7) Uani 1 1 d . U . . .
H7A H 0.2412 0.6889 0.3829 0.030 Uiso 1 1 calc R U . . .
H7B H 0.3752 0.6200 0.4227 0.030 Uiso 1 1 calc R U . . .
C8 C 0.2212(4) 0.6411(3) 0.49825(19) 0.0322(8) Uani 1 1 d . U . . .
H8A H 0.1167 0.6566 0.4916 0.048 Uiso 1 1 calc R U . . .
H8B H 0.2764 0.6980 0.5263 0.048 Uiso 1 1 calc R U . . .
H8C H 0.2410 0.5783 0.5301 0.048 Uiso 1 1 calc R U . . .
C9 C 0.3425(4) 0.5329(2) 0.08502(18) 0.0254(7) Uani 1 1 d . U . . .
H9A H 0.4127 0.5211 0.0469 0.031 Uiso 1 1 calc R U . . .
H9B H 0.2979 0.6012 0.0730 0.031 Uiso 1 1 calc R U . . .
C10 C 0.2242(4) 0.4525(3) 0.0707(2) 0.0322(8) Uani 1 1 d . U . . .
H10A H 0.1698 0.4603 0.0161 0.048 Uiso 1 1 calc R U . . .
H10B H 0.1576 0.4608 0.1105 0.048 Uiso 1 1 calc R U . . .
H10C H 0.2685 0.3842 0.0763 0.048 Uiso 1 1 calc R U . . .
C11 C 0.5184(4) 0.6277(2) 0.18335(19) 0.0261(7) Uani 1 1 d . U . . .
H11A H 0.5735 0.6244 0.2389 0.031 Uiso 1 1 calc R U . . .
H11B H 0.4539 0.6885 0.1808 0.031 Uiso 1 1 calc R U . . .
C12 C 0.6266(4) 0.6442(3) 0.1250(2) 0.0359(9) Uani 1 1 d . U . . .
H12A H 0.5736 0.6553 0.0703 0.054 Uiso 1 1 calc R U . . .
H12B H 0.6891 0.5837 0.1250 0.054 Uiso 1 1 calc R U . . .
H12C H 0.6870 0.7043 0.1418 0.054 Uiso 1 1 calc R U . . .
N2 N 0.2027(3) 0.53552(19) 0.36747(15) 0.0198(5) Uani 1 1 d . U . . .
N3 N 0.4062(3) 0.4154(2) 0.30530(15) 0.0225(5) Uani 1 1 d . U . . .
H3 H 0.3521 0.3528 0.2832 0.027 Uiso 1 1 calc R U . . .
N4 N 0.4235(3) 0.53329(19) 0.16957(15) 0.0200(5) Uani 1 1 d . U . . .
Pd1 Pd 0.29253(2) 0.53856(2) 0.26036(2) 0.01820(8) Uani 1 1 d . U . . .
N1_a N 0.1873(17) 0.6644(10) 0.2178(10) 0.025(2) Uani 0.434(7) 1 d D U P A 1
O1_a O 0.2339(7) 0.7447(5) 0.2470(4) 0.0476(19) Uani 0.434(7) 1 d D U P A 1
O2_a O 0.0773(14) 0.6603(7) 0.1672(8) 0.0476(19) Uani 0.434(7) 1 d D U P A 1
N1A_b N 0.0665(9) 0.6799(5) 0.1723(6) 0.0272(16) Uani 0.566(7) 1 d D U P A 2
O1A_b O 0.1899(10) 0.6754(6) 0.2216(6) 0.0217(16) Uani 0.566(7) 1 d D U P A 2
O2A_b O 0.0158(5) 0.5927(3) 0.1521(3) 0.0362(14) Uani 0.566(7) 1 d D U P A 2
C13 C 0.6078(3) 0.8044(2) 0.40459(19) 0.0235(6) Uani 1 1 d . U . . .
F1 F 0.6550(2) 0.90105(14) 0.40126(11) 0.0318(4) Uani 1 1 d . U . . .
F2 F 0.5585(2) 0.79358(15) 0.47503(11) 0.0353(5) Uani 1 1 d . U . . .
F3 F 0.4948(2) 0.79340(15) 0.34584(11) 0.0327(4) Uani 1 1 d . U . . .
O3 O 0.7914(3) 0.73794(17) 0.31697(14) 0.0316(5) Uani 1 1 d . U . . .
O4 O 0.6775(2) 0.61568(17) 0.39717(13) 0.0286(5) Uani 1 1 d . U . . .
O5 O 0.8593(3) 0.73452(18) 0.46328(15) 0.0348(6) Uani 1 1 d . U . . .
S1 S 0.75174(9) 0.71293(6) 0.39440(5) 0.02337(18) Uani 1 1 d . 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
C1 N2 1.501(4) . ?
C1 C2 1.505(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.481(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.484(4) . ?
C3 C4 1.515(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.508(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.491(4) . ?
C5 C6 1.511(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.504(4) . ?
C7 C8 1.525(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.497(4) . ?
C9 C10 1.510(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.512(4) . ?
C11 C12 1.517(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pd1 2.087(2) . ?
N3 Pd1 2.005(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.084(2) . ?
Pd1 N1_a 1.986(16) . ?
Pd1 O1A_b 2.081(9) . ?
N1_a O1_a 1.208(9) . ?
N1_a O2_a 1.223(9) . ?
N1A_b O2A_b 1.257(8) . ?
N1A_b O1A_b 1.306(6) . ?
C13 F3 1.331(4) . ?
C13 F2 1.334(4) . ?
C13 F1 1.339(4) . ?
C13 S1 1.818(3) . ?
O3 S1 1.436(2) . ?
O4 S1 1.448(2) . ?
O5 S1 1.433(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
N2 C1 C2 110.7(3) . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.8(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.9(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.2(2) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 114.1(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.0(3) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.6(3) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.3(3) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 111.1(2) . . ?
C5 N2 C7 110.0(2) . . ?
C1 N2 C7 110.5(2) . . ?
C5 N2 Pd1 115.14(19) . . ?
C1 N2 Pd1 104.76(17) . . ?
C7 N2 Pd1 105.18(18) . . ?
C2 N3 C3 116.5(3) . . ?
C2 N3 Pd1 107.94(19) . . ?
C3 N3 Pd1 107.75(19) . . ?
C2 N3 H3 108.1 . . ?
C3 N3 H3 108.1 . . ?
Pd1 N3 H3 108.1 . . ?
C9 N4 C4 110.3(2) . . ?
C9 N4 C11 110.1(2) . . ?
C4 N4 C11 110.7(2) . . ?
C9 N4 Pd1 115.05(19) . . ?
C4 N4 Pd1 105.80(17) . . ?
C11 N4 Pd1 104.60(17) . . ?
N1_a Pd1 N3 177.5(4) . . ?
N3 Pd1 O1A_b 174.1(2) . . ?
N1_a Pd1 N4 94.3(5) . . ?
N3 Pd1 N4 85.14(10) . . ?
O1A_b Pd1 N4 95.2(3) . . ?
N1_a Pd1 N2 94.9(5) . . ?
N3 Pd1 N2 85.33(10) . . ?
O1A_b Pd1 N2 93.5(3) . . ?
N4 Pd1 N2 167.68(10) . . ?
O1_a N1_a O2_a 121.8(14) . . ?
O1_a N1_a Pd1 116.5(10) . . ?
O2_a N1_a Pd1 121.6(8) . . ?
O2A_b N1A_b O1A_b 112.7(6) . . ?
N1A_b O1A_b Pd1 123.4(5) . . ?
F3 C13 F2 107.7(3) . . ?
F3 C13 F1 107.3(3) . . ?
F2 C13 F1 107.1(3) . . ?
F3 C13 S1 111.5(2) . . ?
F2 C13 S1 111.6(2) . . ?
F1 C13 S1 111.5(2) . . ?
O5 S1 O3 115.95(15) . . ?
O5 S1 O4 115.02(14) . . ?
O3 S1 O4 114.59(14) . . ?
O5 S1 C13 103.11(14) . . ?
O3 S1 C13 103.14(14) . . ?
O4 S1 C13 102.35(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 -55.8(3) . . . . ?
N3 C3 C4 N4 54.5(3) . . . . ?
C6 C5 N2 C1 -66.5(4) . . . . ?
C6 C5 N2 C7 170.9(3) . . . . ?
C6 C5 N2 Pd1 52.3(3) . . . . ?
C2 C1 N2 C5 161.0(3) . . . . ?
C2 C1 N2 C7 -76.6(3) . . . . ?
C2 C1 N2 Pd1 36.1(3) . . . . ?
C8 C7 N2 C5 56.5(3) . . . . ?
C8 C7 N2 C1 -66.4(3) . . . . ?
C8 C7 N2 Pd1 -179.0(2) . . . . ?
C1 C2 N3 C3 167.6(3) . . . . ?
C1 C2 N3 Pd1 46.3(3) . . . . ?
C4 C3 N3 C2 -169.2(3) . . . . ?
C4 C3 N3 Pd1 -47.8(3) . . . . ?
C10 C9 N4 C4 68.4(3) . . . . ?
C10 C9 N4 C11 -169.0(3) . . . . ?
C10 C9 N4 Pd1 -51.2(3) . . . . ?
C3 C4 N4 C9 -158.5(3) . . . . ?
C3 C4 N4 C11 79.4(3) . . . . ?
C3 C4 N4 Pd1 -33.4(3) . . . . ?
C12 C11 N4 C9 -55.7(4) . . . . ?
C12 C11 N4 C4 66.6(3) . . . . ?
C12 C11 N4 Pd1 -179.9(2) . . . . ?
O2A_b N1A_b O1A_b Pd1 1.1(10) . . . . ?
F3 C13 S1 O5 -178.3(2) . . . . ?
F2 C13 S1 O5 -57.8(3) . . . . ?
F1 C13 S1 O5 61.9(2) . . . . ?
F3 C13 S1 O3 60.7(2) . . . . ?
F2 C13 S1 O3 -178.9(2) . . . . ?
F1 C13 S1 O3 -59.1(2) . . . . ?
F3 C13 S1 O4 -58.6(2) . . . . ?
F2 C13 S1 O4 61.9(2) . . . . ?
F1 C13 S1 O4 -178.4(2) . . . . ?

_refine_diff_density_max         0.661
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.090

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_MS_100K
_database_code_depnum_ccdc_archive 'CCDC 1564442'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2897(4)
_cell_length_b                   13.0472(5)
_cell_length_c                   16.6730(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.853(4)
_cell_angle_gamma                90
_cell_volume                     1996.77(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3329
_cell_measurement_theta_min      4.0060
_cell_measurement_theta_max      28.4930

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82391
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8848
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.359
_diffrn_reflns_theta_max         26.355
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4068
_reflns_number_gt                3397
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0257P)²+1.3253P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4068
_refine_ls_number_parameters     275
_refine_ls_number_restraints     274
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0697
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.037
_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 0.2599(3) 0.4383(2) 0.40976(18) 0.0215(6) Uani 1 1 d . U . . .
H1A H 0.1975 0.3815 0.3891 0.026 Uiso 1 1 calc R U . . .
H1B H 0.2577 0.4443 0.4675 0.026 Uiso 1 1 calc R U . . .
C2 C 0.4138(3) 0.4176(3) 0.39551(18) 0.0231(7) Uani 1 1 d . U . . .
H2A H 0.4788 0.4713 0.4194 0.028 Uiso 1 1 calc R U . . .
H2B H 0.4481 0.3525 0.4193 0.028 Uiso 1 1 calc R U . . .
C3 C 0.5501(3) 0.4178(3) 0.27583(18) 0.0221(6) Uani 1 1 d . U . . .
H3A H 0.6009 0.3532 0.2865 0.027 Uiso 1 1 calc R U . . .
H3B H 0.6111 0.4723 0.3020 0.027 Uiso 1 1 calc R U . . .
C4 C 0.5142(3) 0.4368(2) 0.18523(18) 0.0207(6) Uani 1 1 d . U . . .
H4A H 0.6036 0.4449 0.1625 0.025 Uiso 1 1 calc R U . . .
H4B H 0.4617 0.3785 0.1592 0.025 Uiso 1 1 calc R U . . .
C5 C 0.0418(3) 0.5398(2) 0.35736(18) 0.0218(6) Uani 1 1 d . U . . .
H5A H 0.0103 0.6076 0.3383 0.026 Uiso 1 1 calc R U . . .
H5B H 0.0109 0.5298 0.4098 0.026 Uiso 1 1 calc R U . . .
C6 C -0.0328(4) 0.4612(3) 0.2987(2) 0.0358(9) Uani 1 1 d . U . . .
H6A H 0.0085 0.4631 0.2494 0.054 Uiso 1 1 calc R U . . .
H6B H -0.1350 0.4762 0.2870 0.054 Uiso 1 1 calc R U . . .
H6C H -0.0193 0.3942 0.3225 0.054 Uiso 1 1 calc R U . . .
C7 C 0.2674(3) 0.6272(2) 0.41495(18) 0.0201(6) Uani 1 1 d . U . . .
H7A H 0.2408 0.6878 0.3823 0.024 Uiso 1 1 calc R U . . .
H7B H 0.3727 0.6216 0.4225 0.024 Uiso 1 1 calc R U . . .
C8 C 0.2212(4) 0.6433(3) 0.49768(19) 0.0270(7) Uani 1 1 d . U . . .
H8A H 0.1183 0.6562 0.4910 0.041 Uiso 1 1 calc R U . . .
H8B H 0.2727 0.7009 0.5241 0.041 Uiso 1 1 calc R U . . .
H8C H 0.2434 0.5830 0.5302 0.041 Uiso 1 1 calc R U . . .
C9 C 0.3408(3) 0.5310(2) 0.08442(17) 0.0211(6) Uani 1 1 d . U . . .
H9A H 0.4090 0.5181 0.0470 0.025 Uiso 1 1 calc R U . . .
H9B H 0.2983 0.5981 0.0720 0.025 Uiso 1 1 calc R U . . .
C10 C 0.2213(4) 0.4514(2) 0.0710(2) 0.0269(7) Uani 1 1 d . U . . .
H10A H 0.1697 0.4573 0.0167 0.040 Uiso 1 1 calc R U . . .
H10B H 0.1550 0.4621 0.1090 0.040 Uiso 1 1 calc R U . . .
H10C H 0.2633 0.3842 0.0787 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5158(3) 0.6267(2) 0.18249(18) 0.0213(6) Uani 1 1 d . U . . .
H11A H 0.5702 0.6240 0.2370 0.026 Uiso 1 1 calc R U . . .
H11B H 0.4521 0.6859 0.1798 0.026 Uiso 1 1 calc R U . . .
C12 C 0.6232(4) 0.6434(3) 0.1235(2) 0.0312(8) Uani 1 1 d . U . . .
H12A H 0.5707 0.6571 0.0703 0.047 Uiso 1 1 calc R U . . .
H12B H 0.6816 0.5830 0.1217 0.047 Uiso 1 1 calc R U . . .
H12C H 0.6849 0.7006 0.1411 0.047 Uiso 1 1 calc R U . . .
N2 N 0.2042(3) 0.53536(18) 0.36792(14) 0.0163(5) Uani 1 1 d . U . . .
N3 N 0.4082(3) 0.41532(19) 0.30630(14) 0.0190(5) Uani 1 1 d . U . . .
H3 H 0.3560 0.3532 0.2854 0.023 Uiso 1 1 calc R U . . .
N4 N 0.4224(3) 0.53209(18) 0.16916(14) 0.0174(5) Uani 1 1 d . U . . .
Pd1 Pd 0.29265(2) 0.53710(2) 0.26043(2) 0.01541(8) Uani 1 1 d . U . . .
N1 N 0.1872(14) 0.6629(9) 0.2184(9) 0.0201(11) Uani 0.436(5) 1 d D U P A 1
O1 O 0.2342(6) 0.7444(4) 0.2450(3) 0.0390(14) Uani 0.436(5) 1 d D U P A 1
O2 O 0.0761(10) 0.6605(5) 0.1671(7) 0.0390(14) Uani 0.436(5) 1 d D U P A 1
N1A N 0.0642(13) 0.6798(8) 0.1700(9) 0.0201(11) Uani 0.289(5) 1 d D U P A 2
O1A O 0.1882(17) 0.6711(16) 0.2193(13) 0.0198(10) Uani 0.289(5) 1 d D U P A 2
O2A O 0.0135(8) 0.5906(6) 0.1517(5) 0.0269(13) Uani 0.289(5) 1 d D U P A 2
N1B N 0.0556(11) 0.6280(8) 0.1689(7) 0.0201(11) Uani 0.275(4) 1 d D U P A 3
O1B O 0.1732(16) 0.6656(15) 0.2141(13) 0.0198(10) Uani 0.275(4) 1 d D U P A 3
O2B O -0.0247(8) 0.7012(6) 0.1387(5) 0.0269(13) Uani 0.275(4) 1 d D U P A 3
C13 C 0.6088(3) 0.8047(2) 0.40387(18) 0.0192(5) Uani 1 1 d . U . . .
F1 F 0.65582(19) 0.90118(13) 0.40026(11) 0.0259(4) Uani 1 1 d . U . . .
F2 F 0.5599(2) 0.79357(14) 0.47478(10) 0.0283(4) Uani 1 1 d . U . . .
F3 F 0.49519(19) 0.79340(14) 0.34484(11) 0.0266(4) Uani 1 1 d . U . . .
O3 O 0.7919(2) 0.73800(16) 0.31572(13) 0.0259(5) Uani 1 1 d . U . . .
O4 O 0.6785(2) 0.61581(16) 0.39621(12) 0.0242(5) Uani 1 1 d . U . . .
O5 O 0.8601(2) 0.73448(17) 0.46295(13) 0.0286(5) Uani 1 1 d . U . . .
S1 S 0.75214(8) 0.71294(6) 0.39346(5) 0.01899(17) Uani 1 1 d . 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
C1 N2 1.499(4) . ?
C1 C2 1.510(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.481(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.484(4) . ?
C3 C4 1.516(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.507(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.493(4) . ?
C5 C6 1.510(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.501(4) . ?
C7 C8 1.521(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.497(4) . ?
C9 C10 1.512(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.506(4) . ?
C11 C12 1.521(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N2 Pd1 2.084(2) . ?
N3 Pd1 2.002(2) . ?
N3 H3 0.9800 . ?
N4 Pd1 2.083(2) . ?
Pd1 N1 1.983(13) . ?
Pd1 O1A 2.06(2) . ?
Pd1 O1B 2.092(17) . ?
N1 O1 1.208(9) . ?
N1 O2 1.236(8) . ?
N1A O2A 1.274(9) . ?
N1A O1A 1.313(9) . ?
N1B O2B 1.268(8) . ?
N1B O1B 1.322(9) . ?
C13 F3 1.336(3) . ?
C13 F1 1.337(3) . ?
C13 F2 1.338(3) . ?
C13 S1 1.818(3) . ?
O3 S1 1.439(2) . ?
O4 S1 1.444(2) . ?
O5 S1 1.438(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
N2 C1 C2 110.2(2) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.9(2) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.9(2) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.1(2) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 113.9(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.2(3) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.6(2) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.2(2) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 111.0(2) . . ?
C5 N2 C7 109.7(2) . . ?
C1 N2 C7 110.6(2) . . ?
C5 N2 Pd1 115.05(18) . . ?
C1 N2 Pd1 104.83(16) . . ?
C7 N2 Pd1 105.45(17) . . ?
C2 N3 C3 116.6(2) . . ?
C2 N3 Pd1 107.56(18) . . ?
C3 N3 Pd1 107.69(18) . . ?
C2 N3 H3 108.2 . . ?
C3 N3 H3 108.2 . . ?
Pd1 N3 H3 108.2 . . ?
C9 N4 C11 110.1(2) . . ?
C9 N4 C4 110.5(2) . . ?
C11 N4 C4 110.7(2) . . ?
C9 N4 Pd1 115.08(18) . . ?
C11 N4 Pd1 104.57(17) . . ?
C4 N4 Pd1 105.73(17) . . ?
N1 Pd1 N3 176.7(3) . . ?
N3 Pd1 O1A 174.6(3) . . ?
N1 Pd1 N4 94.5(5) . . ?
N3 Pd1 N4 85.27(9) . . ?
O1A Pd1 N4 94.5(7) . . ?
N1 Pd1 N2 94.2(5) . . ?
N3 Pd1 N2 85.53(9) . . ?
O1A Pd1 N2 93.9(7) . . ?
N4 Pd1 N2 167.79(9) . . ?
N3 Pd1 O1B 179.1(5) . . ?
N4 Pd1 O1B 95.1(7) . . ?
N2 Pd1 O1B 94.0(7) . . ?
O1 N1 O2 119.5(11) . . ?
O1 N1 Pd1 117.9(8) . . ?
O2 N1 Pd1 122.6(7) . . ?
O2A N1A O1A 109.1(10) . . ?
N1A O1A Pd1 127.1(11) . . ?
O2B N1B O1B 109.3(10) . . ?
N1B O1B Pd1 104.9(12) . . ?
F3 C13 F1 107.3(2) . . ?
F3 C13 F2 107.5(2) . . ?
F1 C13 F2 107.4(2) . . ?
F3 C13 S1 111.4(2) . . ?
F1 C13 S1 111.5(2) . . ?
F2 C13 S1 111.5(2) . . ?
O5 S1 O3 115.96(14) . . ?
O5 S1 O4 114.88(13) . . ?
O3 S1 O4 114.61(13) . . ?
O5 S1 C13 102.96(14) . . ?
O3 S1 C13 103.27(13) . . ?
O4 S1 C13 102.54(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 -56.3(3) . . . . ?
N3 C3 C4 N4 54.6(3) . . . . ?
C6 C5 N2 C1 -67.5(3) . . . . ?
C6 C5 N2 C7 169.9(3) . . . . ?
C6 C5 N2 Pd1 51.3(3) . . . . ?
C2 C1 N2 C5 161.2(2) . . . . ?
C2 C1 N2 C7 -76.8(3) . . . . ?
C2 C1 N2 Pd1 36.4(3) . . . . ?
C8 C7 N2 C5 56.3(3) . . . . ?
C8 C7 N2 C1 -66.4(3) . . . . ?
C8 C7 N2 Pd1 -179.2(2) . . . . ?
C1 C2 N3 C3 167.6(2) . . . . ?
C1 C2 N3 Pd1 46.6(3) . . . . ?
C4 C3 N3 C2 -168.6(3) . . . . ?
C4 C3 N3 Pd1 -47.7(3) . . . . ?
C10 C9 N4 C11 -167.8(3) . . . . ?
C10 C9 N4 C4 69.7(3) . . . . ?
C10 C9 N4 Pd1 -49.9(3) . . . . ?
C12 C11 N4 C9 -55.8(3) . . . . ?
C12 C11 N4 C4 66.7(3) . . . . ?
C12 C11 N4 Pd1 -179.9(2) . . . . ?
C3 C4 N4 C9 -158.8(2) . . . . ?
C3 C4 N4 C11 79.0(3) . . . . ?
C3 C4 N4 Pd1 -33.6(3) . . . . ?
O2A N1A O1A Pd1 1.5(18) . . . . ?
O2B N1B O1B Pd1 179.3(9) . . . . ?
F3 C13 S1 O5 -177.9(2) . . . . ?
F1 C13 S1 O5 62.3(2) . . . . ?
F2 C13 S1 O5 -57.8(2) . . . . ?
F3 C13 S1 O3 61.0(2) . . . . ?
F1 C13 S1 O3 -58.8(2) . . . . ?
F2 C13 S1 O3 -178.9(2) . . . . ?
F3 C13 S1 O4 -58.4(2) . . . . ?
F1 C13 S1 O4 -178.2(2) . . . . ?
F2 C13 S1 O4 61.8(2) . . . . ?

_refine_diff_density_max         0.648
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_VT_170K
_database_code_depnum_ccdc_archive 'CCDC 1564444'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2937(5)
_cell_length_b                   12.9717(6)
_cell_length_c                   16.6893(9)
_cell_angle_alpha                90
_cell_angle_beta                 99.227(5)
_cell_angle_gamma                90
_cell_volume                     1985.95(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3186
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.2880
_cell_measurement_theta_min      3.9060

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.099
_shelx_estimated_absorpt_T_min   0.638
_shelx_estimated_absorpt_T_max   0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71290
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8615
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.376
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.000
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4054
_reflns_number_gt                3262
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0300P)²+0.1663P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4054
_refine_ls_number_parameters     270
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0663
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.026
_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 0.2549(4) 0.4364(2) 0.4070(2) 0.0272(7) Uani 1 1 d . U . . .
H1A H 0.1901 0.3783 0.3865 0.033 Uiso 1 1 calc R U . . .
H1B H 0.2549 0.4428 0.4661 0.033 Uiso 1 1 calc R U . . .
C2 C 0.4073(4) 0.4146(2) 0.39164(19) 0.0262(7) Uani 1 1 d . U . . .
H2A H 0.4749 0.4694 0.4156 0.031 Uiso 1 1 calc R U . . .
H2B H 0.4421 0.3477 0.4158 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5405(3) 0.4147(2) 0.2716(2) 0.0240(7) Uani 1 1 d . U . . .
H3A H 0.5916 0.3479 0.2816 0.029 Uiso 1 1 calc R U . . .
H3B H 0.6036 0.4697 0.2993 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5058(3) 0.4359(2) 0.1819(2) 0.0246(7) Uani 1 1 d . U . . .
H4A H 0.4525 0.3765 0.1542 0.029 Uiso 1 1 calc R U . . .
H4B H 0.5975 0.4446 0.1597 0.029 Uiso 1 1 calc R U . . .
C5 C 0.0368(3) 0.5388(3) 0.3560(2) 0.0277(7) Uani 1 1 d . U . . .
H5A H 0.0043 0.6068 0.3328 0.033 Uiso 1 1 calc R U . . .
H5B H 0.0076 0.5341 0.4104 0.033 Uiso 1 1 calc R U . . .
C6 C -0.0408(4) 0.4553(3) 0.3026(2) 0.0409(9) Uani 1 1 d . U . . .
H6A H 0.0059 0.4467 0.2544 0.061 Uiso 1 1 calc R U . . .
H6B H -0.1432 0.4747 0.2860 0.061 Uiso 1 1 calc R U . . .
H6C H -0.0355 0.3903 0.3329 0.061 Uiso 1 1 calc R U . . .
C7 C 0.2638(3) 0.6261(2) 0.4120(2) 0.0245(7) Uani 1 1 d . U . . .
H7A H 0.2348 0.6883 0.3791 0.029 Uiso 1 1 calc R U . . .
H7B H 0.3713 0.6205 0.4183 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2225(4) 0.6420(3) 0.4955(2) 0.0320(8) Uani 1 1 d . U . . .
H8A H 0.1180 0.6568 0.4900 0.048 Uiso 1 1 calc R U . . .
H8B H 0.2781 0.7000 0.5224 0.048 Uiso 1 1 calc R U . . .
H8C H 0.2448 0.5794 0.5280 0.048 Uiso 1 1 calc R U . . .
C9 C 0.3340(4) 0.5323(2) 0.0818(2) 0.0262(7) Uani 1 1 d . U . . .
H9A H 0.4048 0.5242 0.0438 0.031 Uiso 1 1 calc R U . . .
H9B H 0.2860 0.6002 0.0709 0.031 Uiso 1 1 calc R U . . .
C10 C 0.2198(4) 0.4487(3) 0.0647(2) 0.0328(8) Uani 1 1 d . U . . .
H10A H 0.1620 0.4597 0.0109 0.049 Uiso 1 1 calc R U . . .
H10B H 0.1557 0.4510 0.1060 0.049 Uiso 1 1 calc R U . . .
H10C H 0.2677 0.3813 0.0662 0.049 Uiso 1 1 calc R U . . .
C11 C 0.5087(3) 0.6269(2) 0.1815(2) 0.0245(7) Uani 1 1 d . U . . .
H11A H 0.5631 0.6230 0.2375 0.029 Uiso 1 1 calc R U . . .
H11B H 0.4442 0.6880 0.1788 0.029 Uiso 1 1 calc R U . . .
C12 C 0.6182(4) 0.6441(3) 0.1237(2) 0.0348(9) Uani 1 1 d . U . . .
H12A H 0.5657 0.6548 0.0685 0.052 Uiso 1 1 calc R U . . .
H12B H 0.6814 0.5836 0.1245 0.052 Uiso 1 1 calc R U . . .
H12C H 0.6776 0.7050 0.1409 0.052 Uiso 1 1 calc R U . . .
N2 N 0.1987(3) 0.53374(18) 0.36546(16) 0.0199(5) Uani 1 1 d . U . . .
N3 N 0.3991(3) 0.41202(19) 0.30188(15) 0.0203(5) Uani 1 1 d . U . . .
H3 H 0.3447 0.3487 0.2804 0.024 Uiso 1 1 calc R U . . .
N4 N 0.4143(3) 0.53183(18) 0.16597(16) 0.0198(5) Uani 1 1 d . U . . .
Pd1 Pd 0.28510(2) 0.53649(2) 0.25745(2) 0.01705(9) Uani 1 1 d D U . . .
N1_a N 0.166(3) 0.6612(17) 0.217(2) 0.018(4) Uani 0.053(5) 1 d D U P A 1
O1_a O 0.215(4) 0.7432(15) 0.241(2) 0.017(7) Uani 0.053(5) 1 d D U P A 1
O2_a O 0.052(4) 0.653(3) 0.172(4) 0.017(7) Uani 0.053(5) 1 d D U P A 1
N1A_b N 0.0637(4) 0.6783(2) 0.1716(3) 0.0331(10) Uani 0.947(5) 1 d D U P A 2
O1A_b O 0.1882(3) 0.67491(18) 0.22014(17) 0.0251(6) Uani 0.947(5) 1 d D U P A 2
O2A_b O 0.0117(3) 0.5937(2) 0.15091(18) 0.0442(9) Uani 0.947(5) 1 d D U P A 2
C13 C 0.6059(3) 0.8011(2) 0.4026(2) 0.0253(6) Uani 1 1 d . U . . .
F1 F 0.6515(2) 0.89794(13) 0.39882(12) 0.0342(5) Uani 1 1 d . U . . .
F2 F 0.5572(2) 0.78981(15) 0.47304(12) 0.0381(5) Uani 1 1 d . U . . .
F3 F 0.49147(19) 0.78889(14) 0.34339(12) 0.0342(5) Uani 1 1 d . U . . .
O3 O 0.7879(3) 0.73504(17) 0.31443(15) 0.0350(6) Uani 1 1 d . U . . .
O4 O 0.6770(2) 0.61160(17) 0.39526(14) 0.0310(5) Uani 1 1 d . U . . .
O5 O 0.8580(2) 0.73224(18) 0.46148(16) 0.0380(6) Uani 1 1 d . U . . .
S1 S 0.74995(8) 0.70983(6) 0.39217(5) 0.02420(19) Uani 1 1 d . 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
C1 N2 1.494(4) . ?
C1 C2 1.506(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.488(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.482(4) . ?
C3 C4 1.504(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.507(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.490(4) . ?
C5 C6 1.510(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.501(4) . ?
C7 C8 1.517(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.481(4) . ?
C9 C10 1.513(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.512(4) . ?
C11 C12 1.527(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pd1 2.088(2) . ?
N3 Pd1 2.007(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.089(2) . ?
Pd1 N1_a 2.014(15) . ?
Pd1 O1A_b 2.060(2) . ?
N1_a O1_a 1.198(10) . ?
N1_a O2_a 1.201(10) . ?
N1A_b O2A_b 1.226(4) . ?
N1A_b O1A_b 1.303(3) . ?
C13 F1 1.331(4) . ?
C13 F2 1.334(4) . ?
C13 F3 1.340(4) . ?
C13 S1 1.816(3) . ?
O3 S1 1.436(2) . ?
O4 S1 1.448(2) . ?
O5 S1 1.435(3) . ?

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
N2 C1 C2 110.3(2) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.1(3) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.5(3) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C3 C4 N4 110.6(2) . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 114.2(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.4(3) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 114.0(3) . . ?
N4 C9 H9A 108.7 . . ?
C10 C9 H9A 108.7 . . ?
N4 C9 H9B 108.7 . . ?
C10 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.0(3) . . ?
N4 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N4 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 111.0(2) . . ?
C5 N2 C7 109.6(2) . . ?
C1 N2 C7 110.6(3) . . ?
C5 N2 Pd1 115.4(2) . . ?
C1 N2 Pd1 105.14(17) . . ?
C7 N2 Pd1 104.75(17) . . ?
C3 N3 C2 116.0(3) . . ?
C3 N3 Pd1 107.42(18) . . ?
C2 N3 Pd1 107.00(18) . . ?
C3 N3 H3 108.7 . . ?
C2 N3 H3 108.7 . . ?
Pd1 N3 H3 108.7 . . ?
C9 N4 C4 110.8(2) . . ?
C9 N4 C11 110.5(2) . . ?
C4 N4 C11 110.4(2) . . ?
C9 N4 Pd1 115.56(18) . . ?
C4 N4 Pd1 105.59(17) . . ?
C11 N4 Pd1 103.69(17) . . ?
N3 Pd1 N1_a 177.4(10) . . ?
N3 Pd1 O1A_b 172.90(10) . . ?
N3 Pd1 N2 85.44(10) . . ?
N1_a Pd1 N2 91.9(10) . . ?
O1A_b Pd1 N2 93.79(10) . . ?
N3 Pd1 N4 85.15(9) . . ?
N1_a Pd1 N4 97.5(10) . . ?
O1A_b Pd1 N4 94.52(10) . . ?
N2 Pd1 N4 167.44(10) . . ?
O1_a N1_a O2_a 122.4(14) . . ?
O1_a N1_a Pd1 116.3(13) . . ?
O2_a N1_a Pd1 121.3(13) . . ?
O2A_b N1A_b O1A_b 114.6(3) . . ?
N1A_b O1A_b Pd1 121.3(2) . . ?
F1 C13 F2 107.5(3) . . ?
F1 C13 F3 107.3(3) . . ?
F2 C13 F3 107.2(2) . . ?
F1 C13 S1 111.5(2) . . ?
F2 C13 S1 111.9(2) . . ?
F3 C13 S1 111.2(2) . . ?
O5 S1 O3 116.16(15) . . ?
O5 S1 O4 114.87(15) . . ?
O3 S1 O4 114.63(14) . . ?
O5 S1 C13 102.83(15) . . ?
O3 S1 C13 103.29(15) . . ?
O4 S1 C13 102.35(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 -56.1(3) . . . . ?
N3 C3 C4 N4 54.2(3) . . . . ?
C6 C5 N2 C1 -63.4(4) . . . . ?
C6 C5 N2 C7 174.1(3) . . . . ?
C6 C5 N2 Pd1 56.1(3) . . . . ?
C2 C1 N2 C5 161.0(3) . . . . ?
C2 C1 N2 C7 -77.0(3) . . . . ?
C2 C1 N2 Pd1 35.5(3) . . . . ?
C8 C7 N2 C5 57.1(4) . . . . ?
C8 C7 N2 C1 -65.6(3) . . . . ?
C8 C7 N2 Pd1 -178.4(2) . . . . ?
C4 C3 N3 C2 -167.3(2) . . . . ?
C4 C3 N3 Pd1 -47.7(3) . . . . ?
C1 C2 N3 C3 167.0(2) . . . . ?
C1 C2 N3 Pd1 47.2(3) . . . . ?
C10 C9 N4 C4 66.2(3) . . . . ?
C10 C9 N4 C11 -171.2(3) . . . . ?
C10 C9 N4 Pd1 -53.9(3) . . . . ?
C3 C4 N4 C9 -158.5(2) . . . . ?
C3 C4 N4 C11 78.8(3) . . . . ?
C3 C4 N4 Pd1 -32.6(3) . . . . ?
C12 C11 N4 C9 -56.3(3) . . . . ?
C12 C11 N4 C4 66.7(4) . . . . ?
C12 C11 N4 Pd1 179.3(2) . . . . ?
O2A_b N1A_b O1A_b Pd1 -0.1(5) . . . . ?
F1 C13 S1 O5 62.3(3) . . . . ?
F2 C13 S1 O5 -58.1(3) . . . . ?
F3 C13 S1 O5 -177.9(2) . . . . ?
F1 C13 S1 O3 -58.9(3) . . . . ?
F2 C13 S1 O3 -179.3(2) . . . . ?
F3 C13 S1 O3 60.8(2) . . . . ?
F1 C13 S1 O4 -178.2(2) . . . . ?
F2 C13 S1 O4 61.3(3) . . . . ?
F3 C13 S1 O4 -58.5(2) . . . . ?

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
N3 H3 N1_a 1.00 2.44 3.315(19) 146.5 2_545
N3 H3 O1_a 1.00 1.50 2.487(19) 169.0 2_545
N3 H3 N1A_b 1.00 2.46 3.076(4) 119.5 2_545
N3 H3 O1A_b 1.00 2.28 3.187(3) 151.0 2_545

_refine_diff_density_max         0.802
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.095

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_VT_100K
_database_code_depnum_ccdc_archive 'CCDC 1564443'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2812(4)
_cell_length_b                   13.0534(6)
_cell_length_c                   16.6886(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.782(4)
_cell_angle_gamma                90
_cell_volume                     1998.14(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3348
_cell_measurement_theta_min      4.0020
_cell_measurement_theta_max      28.8180

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.092
_shelx_estimated_absorpt_T_min   0.639
_shelx_estimated_absorpt_T_max   0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8854
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.357
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4072
_reflns_number_gt                3385
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0275P)²+1.2115P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4072
_refine_ls_number_parameters     275
_refine_ls_number_restraints     274
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0730
_refine_ls_wR_factor_gt          0.0674
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.041
_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 0.2592(4) 0.4380(2) 0.40934(19) 0.0232(7) Uani 1 1 d . U . . .
H1A H 0.1953 0.3803 0.3882 0.028 Uiso 1 1 calc R U . . .
H1B H 0.2570 0.4439 0.4683 0.028 Uiso 1 1 calc R U . . .
C2 C 0.4125(4) 0.4170(3) 0.39511(18) 0.0244(7) Uani 1 1 d . U . . .
H2A H 0.4792 0.4714 0.4198 0.029 Uiso 1 1 calc R U . . .
H2B H 0.4468 0.3503 0.4191 0.029 Uiso 1 1 calc R U . . .
C3 C 0.5500(3) 0.4177(3) 0.27592(18) 0.0232(7) Uani 1 1 d . U . . .
H3A H 0.6016 0.3516 0.2865 0.028 Uiso 1 1 calc R U . . .
H3B H 0.6124 0.4731 0.3029 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5141(4) 0.4375(2) 0.18512(18) 0.0226(7) Uani 1 1 d . U . . .
H4A H 0.6055 0.4456 0.1620 0.027 Uiso 1 1 calc R U . . .
H4B H 0.4601 0.3783 0.1583 0.027 Uiso 1 1 calc R U . . .
C5 C 0.0410(3) 0.5403(3) 0.35706(19) 0.0237(7) Uani 1 1 d . U . . .
H5A H 0.0094 0.6094 0.3372 0.028 Uiso 1 1 calc R U . . .
H5B H 0.0093 0.5307 0.4106 0.028 Uiso 1 1 calc R U . . .
C6 C -0.0341(4) 0.4617(3) 0.2990(2) 0.0395(9) Uani 1 1 d . U . . .
H6A H 0.0082 0.4629 0.2487 0.059 Uiso 1 1 calc R U . . .
H6B H -0.1384 0.4776 0.2870 0.059 Uiso 1 1 calc R U . . .
H6C H -0.0209 0.3935 0.3236 0.059 Uiso 1 1 calc R U . . .
C7 C 0.2670(3) 0.6273(2) 0.41513(19) 0.0224(6) Uani 1 1 d . U . . .
H7A H 0.2394 0.6893 0.3822 0.027 Uiso 1 1 calc R U . . .
H7B H 0.3746 0.6218 0.4226 0.027 Uiso 1 1 calc R U . . .
C8 C 0.2211(4) 0.6425(3) 0.49786(19) 0.0295(8) Uani 1 1 d . U . . .
H8A H 0.1163 0.6568 0.4912 0.044 Uiso 1 1 calc R U . . .
H8B H 0.2750 0.7003 0.5254 0.044 Uiso 1 1 calc R U . . .
H8C H 0.2425 0.5803 0.5304 0.044 Uiso 1 1 calc R U . . .
C9 C 0.3419(4) 0.5316(2) 0.08470(18) 0.0221(6) Uani 1 1 d . U . . .
H9A H 0.4118 0.5189 0.0466 0.027 Uiso 1 1 calc R U . . .
H9B H 0.2981 0.6000 0.0722 0.027 Uiso 1 1 calc R U . . .
C10 C 0.2224(4) 0.4516(3) 0.0708(2) 0.0281(7) Uani 1 1 d . U . . .
H10A H 0.1675 0.4597 0.0162 0.042 Uiso 1 1 calc R U . . .
H10B H 0.1566 0.4603 0.1109 0.042 Uiso 1 1 calc R U . . .
H10C H 0.2660 0.3831 0.0763 0.042 Uiso 1 1 calc R U . . .
C11 C 0.5169(4) 0.6275(2) 0.18262(18) 0.0224(7) Uani 1 1 d . U . . .
H11A H 0.5720 0.6249 0.2383 0.027 Uiso 1 1 calc R U . . .
H11B H 0.4518 0.6879 0.1796 0.027 Uiso 1 1 calc R U . . .
C12 C 0.6242(4) 0.6437(3) 0.1241(2) 0.0319(8) Uani 1 1 d . U . . .
H12A H 0.5709 0.6562 0.0697 0.048 Uiso 1 1 calc R U . . .
H12B H 0.6852 0.5826 0.1233 0.048 Uiso 1 1 calc R U . . .
H12C H 0.6860 0.7030 0.1415 0.048 Uiso 1 1 calc R U . . .
N2 N 0.2039(3) 0.53550(19) 0.36776(15) 0.0176(5) Uani 1 1 d . U . . .
N3 N 0.4076(3) 0.4153(2) 0.30600(14) 0.0195(5) Uani 1 1 d . U . . .
H3 H 0.3543 0.3522 0.2843 0.023 Uiso 1 1 calc R U . . .
N4 N 0.4233(3) 0.53268(19) 0.16943(15) 0.0184(5) Uani 1 1 d . U . . .
Pd1 Pd 0.29261(2) 0.53767(2) 0.26040(2) 0.01640(8) Uani 1 1 d . U . . .
N1_a N 0.1880(15) 0.6629(9) 0.2181(9) 0.0229(11) Uani 0.430(5) 1 d D U P A 1
O1_a O 0.2336(7) 0.7444(4) 0.2458(4) 0.0423(16) Uani 0.430(5) 1 d D U P A 1
O2_a O 0.0772(11) 0.6606(6) 0.1670(8) 0.0423(16) Uani 0.430(5) 1 d D U P A 1
N1A_b N 0.0634(10) 0.6798(6) 0.1710(7) 0.0229(11) Uani 0.398(5) 1 d D U P A 2
O1A_b O 0.1881(14) 0.6715(13) 0.2204(11) 0.0210(9) Uani 0.398(5) 1 d D U P A 2
O2A_b O 0.0145(7) 0.5912(4) 0.1520(4) 0.0318(13) Uani 0.398(5) 1 d D U P A 2
N1B_c N 0.0583(19) 0.6303(12) 0.1701(12) 0.0229(11) Uani 0.172(5) 1 d D U P A 3
O1B_c O 0.174(3) 0.670(3) 0.215(2) 0.0210(9) Uani 0.172(5) 1 d D U P A 3
O2B_c O -0.0230(13) 0.7041(10) 0.1387(8) 0.0318(13) Uani 0.172(5) 1 d D U P A 3
C13 C 0.6081(3) 0.8046(2) 0.40405(19) 0.0211(5) Uani 1 1 d . U . . .
F1 F 0.6556(2) 0.90096(13) 0.40082(11) 0.0281(4) Uani 1 1 d . U . . .
F2 F 0.5592(2) 0.79378(15) 0.47490(11) 0.0302(4) Uani 1 1 d . U . . .
F3 F 0.4951(2) 0.79353(14) 0.34511(11) 0.0284(4) Uani 1 1 d . U . . .
O3 O 0.7914(3) 0.73790(18) 0.31620(13) 0.0284(5) Uani 1 1 d . U . . .
O4 O 0.6783(2) 0.61574(17) 0.39657(13) 0.0253(5) Uani 1 1 d . U . . .
O5 O 0.8597(3) 0.73450(18) 0.46315(14) 0.0314(6) Uani 1 1 d . U . . .
S1 S 0.75198(8) 0.71296(6) 0.39387(5) 0.02078(18) Uani 1 1 d . 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
C1 N2 1.502(4) . ?
C1 C2 1.503(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.481(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.483(4) . ?
C3 C4 1.523(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.501(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.496(4) . ?
C5 C6 1.506(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.504(4) . ?
C7 C8 1.519(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.498(4) . ?
C9 C10 1.515(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.508(4) . ?
C11 C12 1.512(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pd1 2.083(2) . ?
N3 Pd1 2.006(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.084(2) . ?
Pd1 N1_a 1.975(14) . ?
Pd1 O1A_b 2.059(17) . ?
Pd1 O1B_c 2.13(3) . ?
N1_a O1_a 1.210(9) . ?
N1_a O2_a 1.232(8) . ?
N1A_b O2A_b 1.265(8) . ?
N1A_b O1A_b 1.318(8) . ?
N1B_c O2B_c 1.285(10) . ?
N1B_c O1B_c 1.314(10) . ?
C13 F3 1.332(3) . ?
C13 F2 1.337(3) . ?
C13 F1 1.337(4) . ?
C13 S1 1.819(3) . ?
O3 S1 1.437(2) . ?
O4 S1 1.446(2) . ?
O5 S1 1.436(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
N2 C1 C2 110.3(3) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.1(3) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.6(2) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.2(2) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 114.1(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.2(3) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.7(2) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.3(3) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 111.0(2) . . ?
C5 N2 C7 109.6(2) . . ?
C1 N2 C7 110.7(2) . . ?
C5 N2 Pd1 114.94(19) . . ?
C1 N2 Pd1 104.87(17) . . ?
C7 N2 Pd1 105.54(18) . . ?
C2 N3 C3 116.6(2) . . ?
C2 N3 Pd1 107.56(19) . . ?
C3 N3 Pd1 107.71(18) . . ?
C2 N3 H3 108.3 . . ?
C3 N3 H3 108.3 . . ?
Pd1 N3 H3 108.3 . . ?
C9 N4 C4 110.2(2) . . ?
C9 N4 C11 110.0(2) . . ?
C4 N4 C11 111.0(2) . . ?
C9 N4 Pd1 114.97(18) . . ?
C4 N4 Pd1 105.81(17) . . ?
C11 N4 Pd1 104.73(17) . . ?
N1_a Pd1 N3 176.9(3) . . ?
N3 Pd1 O1A_b 174.8(3) . . ?
N1_a Pd1 N2 94.7(5) . . ?
N3 Pd1 N2 85.42(10) . . ?
O1A_b Pd1 N2 93.6(6) . . ?
N1_a Pd1 N4 94.3(5) . . ?
N3 Pd1 N4 85.19(10) . . ?
O1A_b Pd1 N4 95.1(6) . . ?
N2 Pd1 N4 167.59(10) . . ?
N3 Pd1 O1B_c 178.4(7) . . ?
N2 Pd1 O1B_c 94.0(11) . . ?
N4 Pd1 O1B_c 95.2(11) . . ?
O1_a N1_a O2_a 119.4(11) . . ?
O1_a N1_a Pd1 117.8(9) . . ?
O2_a N1_a Pd1 122.7(7) . . ?
O2A_b N1A_b O1A_b 109.2(9) . . ?
N1A_b O1A_b Pd1 126.7(9) . . ?
O2B_c N1B_c O1B_c 108.3(11) . . ?
N1B_c O1B_c Pd1 102.6(18) . . ?
F3 C13 F2 107.8(2) . . ?
F3 C13 F1 107.4(2) . . ?
F2 C13 F1 107.1(3) . . ?
F3 C13 S1 111.5(2) . . ?
F2 C13 S1 111.5(2) . . ?
F1 C13 S1 111.3(2) . . ?
O5 S1 O3 116.09(15) . . ?
O5 S1 O4 114.93(14) . . ?
O3 S1 O4 114.45(14) . . ?
O5 S1 C13 103.11(14) . . ?
O3 S1 C13 103.11(14) . . ?
O4 S1 C13 102.51(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 -56.1(3) . . . . ?
N3 C3 C4 N4 54.8(3) . . . . ?
C6 C5 N2 C1 -66.9(3) . . . . ?
C6 C5 N2 C7 170.5(3) . . . . ?
C6 C5 N2 Pd1 51.9(3) . . . . ?
C2 C1 N2 C5 161.0(3) . . . . ?
C2 C1 N2 C7 -77.1(3) . . . . ?
C2 C1 N2 Pd1 36.3(3) . . . . ?
C8 C7 N2 C5 56.8(3) . . . . ?
C8 C7 N2 C1 -66.0(3) . . . . ?
C8 C7 N2 Pd1 -178.9(2) . . . . ?
C1 C2 N3 C3 167.5(3) . . . . ?
C1 C2 N3 Pd1 46.5(3) . . . . ?
C4 C3 N3 C2 -168.6(3) . . . . ?
C4 C3 N3 Pd1 -47.7(3) . . . . ?
C10 C9 N4 C4 69.2(3) . . . . ?
C10 C9 N4 C11 -168.1(3) . . . . ?
C10 C9 N4 Pd1 -50.3(3) . . . . ?
C3 C4 N4 C9 -158.7(3) . . . . ?
C3 C4 N4 C11 79.3(3) . . . . ?
C3 C4 N4 Pd1 -33.8(3) . . . . ?
C12 C11 N4 C9 -56.0(4) . . . . ?
C12 C11 N4 C4 66.3(3) . . . . ?
C12 C11 N4 Pd1 180.0(2) . . . . ?
O2A_b N1A_b O1A_b Pd1 0.9(16) . . . . ?
O2B_c N1B_c O1B_c Pd1 180.0(12) . . . . ?
F3 C13 S1 O5 -178.2(2) . . . . ?
F2 C13 S1 O5 -57.6(2) . . . . ?
F1 C13 S1 O5 61.9(2) . . . . ?
F3 C13 S1 O3 60.6(2) . . . . ?
F2 C13 S1 O3 -178.8(2) . . . . ?
F1 C13 S1 O3 -59.3(2) . . . . ?
F3 C13 S1 O4 -58.5(2) . . . . ?
F2 C13 S1 O4 62.1(2) . . . . ?
F1 C13 S1 O4 -178.5(2) . . . . ?

_refine_diff_density_max         0.601
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.092

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_VT_190K
_database_code_depnum_ccdc_archive 'CCDC 1564445'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2479(4)
_cell_length_b                   13.1454(5)
_cell_length_c                   17.0808(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.510(4)
_cell_angle_gamma                90
_cell_volume                     2063.08(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    3096
_cell_measurement_theta_min      3.9080
_cell_measurement_theta_max      29.1880

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.058
_shelx_estimated_absorpt_T_min   0.648
_shelx_estimated_absorpt_T_max   0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9006
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.324
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4211
_reflns_number_gt                3360
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0276P)²+0.4595P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4211
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_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 0.2579(4) 0.4379(2) 0.4079(2) 0.0321(8) Uani 1 1 d . . . . .
H1A H 0.1954 0.3824 0.3839 0.038 Uiso 1 1 calc R U . . .
H1B H 0.2479 0.4398 0.4649 0.038 Uiso 1 1 calc R U . . .
C2 C 0.4143(3) 0.4173(2) 0.39597(19) 0.0299(7) Uani 1 1 d . . . . .
H2A H 0.4792 0.4692 0.4234 0.036 Uiso 1 1 calc R U . . .
H2B H 0.4447 0.3493 0.4166 0.036 Uiso 1 1 calc R U . . .
C3 C 0.5657(3) 0.4245(2) 0.2817(2) 0.0297(8) Uani 1 1 d . . . . .
H3A H 0.6158 0.3584 0.2913 0.036 Uiso 1 1 calc R U . . .
H3B H 0.6267 0.4786 0.3088 0.036 Uiso 1 1 calc R U . . .
C4 C 0.5378(4) 0.4458(2) 0.1950(2) 0.0324(8) Uani 1 1 d . . . . .
H4A H 0.6318 0.4541 0.1732 0.039 Uiso 1 1 calc R U . . .
H4B H 0.4862 0.3873 0.1682 0.039 Uiso 1 1 calc R U . . .
C5 C 0.0470(3) 0.5430(3) 0.3583(2) 0.0384(9) Uani 1 1 d . . . . .
H5A H 0.0176 0.6139 0.3447 0.046 Uiso 1 1 calc R U . . .
H5B H 0.0082 0.5255 0.4083 0.046 Uiso 1 1 calc R U . . .
C6 C -0.0206(4) 0.4735(3) 0.2945(3) 0.0551(11) Uani 1 1 d . . . . .
H6A H 0.0232 0.4862 0.2458 0.083 Uiso 1 1 calc R U . . .
H6B H -0.1256 0.4863 0.2854 0.083 Uiso 1 1 calc R U . . .
H6C H -0.0035 0.4026 0.3107 0.083 Uiso 1 1 calc R U . . .
C7 C 0.2696(3) 0.6244(2) 0.42115(19) 0.0306(7) Uani 1 1 d . . . . .
H7A H 0.2464 0.6885 0.3919 0.037 Uiso 1 1 calc R U . . .
H7B H 0.3769 0.6179 0.4290 0.037 Uiso 1 1 calc R U . . .
C8 C 0.2151(4) 0.6335(3) 0.5018(2) 0.0461(10) Uani 1 1 d . . . . .
H8A H 0.1101 0.6464 0.4951 0.069 Uiso 1 1 calc R U . . .
H8B H 0.2652 0.6900 0.5309 0.069 Uiso 1 1 calc R U . . .
H8C H 0.2351 0.5701 0.5312 0.069 Uiso 1 1 calc R U . . .
C9 C 0.3716(4) 0.5383(3) 0.0973(2) 0.0366(8) Uani 1 1 d . . . . .
H9A H 0.4429 0.5215 0.0602 0.044 Uiso 1 1 calc R U . . .
H9B H 0.3330 0.6071 0.0838 0.044 Uiso 1 1 calc R U . . .
C10 C 0.2480(4) 0.4629(3) 0.0862(2) 0.0469(10) Uani 1 1 d . . . . .
H10A H 0.2045 0.4640 0.0312 0.070 Uiso 1 1 calc R U . . .
H10B H 0.1741 0.4812 0.1206 0.070 Uiso 1 1 calc R U . . .
H10C H 0.2851 0.3945 0.0997 0.070 Uiso 1 1 calc R U . . .
C11 C 0.5422(4) 0.6333(2) 0.1917(2) 0.0347(8) Uani 1 1 d . . . . .
H11A H 0.5935 0.6307 0.2458 0.042 Uiso 1 1 calc R U . . .
H11B H 0.4781 0.6938 0.1885 0.042 Uiso 1 1 calc R U . . .
C12 C 0.6553(4) 0.6476(3) 0.1341(3) 0.0588(12) Uani 1 1 d . . . . .
H12A H 0.6059 0.6610 0.0813 0.088 Uiso 1 1 calc R U . . .
H12B H 0.7143 0.5858 0.1330 0.088 Uiso 1 1 calc R U . . .
H12C H 0.7183 0.7053 0.1511 0.088 Uiso 1 1 calc R U . . .
N1 N 0.2004(3) 0.6704(2) 0.22606(17) 0.0312(6) Uani 1 1 d . . . . .
N2 N 0.2094(3) 0.53765(18) 0.37078(15) 0.0246(6) Uani 1 1 d . . . . .
N3 N 0.4200(2) 0.42218(17) 0.31009(15) 0.0209(5) Uani 1 1 d . . . . .
H3 H 0.3679 0.3610 0.2864 0.025 Uiso 1 1 calc R U . . .
N4 N 0.4482(3) 0.54019(18) 0.17911(15) 0.0261(6) Uani 1 1 d . . . . .
O1 O 0.2390(3) 0.75250(19) 0.25494(18) 0.0630(9) Uani 1 1 d . . . . .
O2 O 0.0976(3) 0.6684(2) 0.17539(19) 0.0727(10) Uani 1 1 d . . . . .
Pd1 Pd 0.30977(2) 0.54470(2) 0.26755(2) 0.01983(8) Uani 1 1 d . . . . .
C13 C 0.6109(4) 0.8122(3) 0.4130(2) 0.0341(8) Uani 1 1 d . . . . .
F1 F 0.6604(2) 0.90696(14) 0.41080(14) 0.0498(6) Uani 1 1 d . . . . .
F2 F 0.5559(2) 0.80091(16) 0.48095(13) 0.0567(6) Uani 1 1 d . . . . .
F3 F 0.5015(2) 0.80343(17) 0.35607(14) 0.0562(6) Uani 1 1 d . . . . .
O3 O 0.7949(3) 0.74313(18) 0.32547(15) 0.0471(7) Uani 1 1 d . . . . .
O4 O 0.6749(3) 0.62381(16) 0.40405(14) 0.0397(6) Uani 1 1 d . . . . .
O5 O 0.8574(3) 0.7382(2) 0.46738(17) 0.0551(7) Uani 1 1 d . . . . .
S1 S 0.75164(9) 0.71903(6) 0.40130(5) 0.0321(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.503(4) . ?
C1 C2 1.507(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.475(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.483(3) . ?
C3 C4 1.500(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.500(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.495(4) . ?
C5 C6 1.503(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.497(4) . ?
C7 C8 1.524(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.493(4) . ?
C9 C10 1.509(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.502(4) . ?
C11 C12 1.527(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 O2 1.211(4) . ?
N1 O1 1.223(4) . ?
N1 Pd1 2.023(3) . ?
N2 Pd1 2.086(2) . ?
N3 Pd1 1.998(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.089(2) . ?
C13 F3 1.326(4) . ?
C13 F2 1.327(4) . ?
C13 F1 1.329(4) . ?
C13 S1 1.815(3) . ?
O3 S1 1.433(3) . ?
O4 S1 1.442(2) . ?
O5 S1 1.430(3) . ?

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
N2 C1 C2 110.2(2) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.6(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.4(2) . . ?
N3 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
N3 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
N4 C4 C3 111.3(2) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 113.8(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.1(3) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.6(3) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 115.8(3) . . ?
N4 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N4 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 N1 O1 118.4(3) . . ?
O2 N1 Pd1 123.6(2) . . ?
O1 N1 Pd1 117.9(2) . . ?
C5 N2 C7 110.4(2) . . ?
C5 N2 C1 110.4(2) . . ?
C7 N2 C1 110.4(3) . . ?
C5 N2 Pd1 114.4(2) . . ?
C7 N2 Pd1 106.25(17) . . ?
C1 N2 Pd1 104.78(17) . . ?
C2 N3 C3 117.6(2) . . ?
C2 N3 Pd1 108.78(18) . . ?
C3 N3 Pd1 108.02(18) . . ?
C2 N3 H3 107.4 . . ?
C3 N3 H3 107.4 . . ?
Pd1 N3 H3 107.4 . . ?
C9 N4 C4 110.5(2) . . ?
C9 N4 C11 110.7(2) . . ?
C4 N4 C11 110.5(2) . . ?
C9 N4 Pd1 114.35(19) . . ?
C4 N4 Pd1 105.29(18) . . ?
C11 N4 Pd1 105.37(18) . . ?
N3 Pd1 N1 178.90(11) . . ?
N3 Pd1 N2 85.09(9) . . ?
N1 Pd1 N2 94.58(10) . . ?
N3 Pd1 N4 84.88(10) . . ?
N1 Pd1 N4 95.32(10) . . ?
N2 Pd1 N4 167.99(10) . . ?
F3 C13 F2 107.2(3) . . ?
F3 C13 F1 107.3(3) . . ?
F2 C13 F1 107.3(3) . . ?
F3 C13 S1 111.0(2) . . ?
F2 C13 S1 111.8(2) . . ?
F1 C13 S1 112.1(2) . . ?
O5 S1 O3 116.00(17) . . ?
O5 S1 O4 114.99(16) . . ?
O3 S1 O4 114.21(15) . . ?
O5 S1 C13 103.25(16) . . ?
O3 S1 C13 103.13(16) . . ?
O4 S1 C13 102.73(15) . . ?

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
N2 C1 C2 N3 -55.9(3) . . . . ?
N3 C3 C4 N4 54.3(3) . . . . ?
C6 C5 N2 C7 167.2(3) . . . . ?
C6 C5 N2 C1 -70.5(4) . . . . ?
C6 C5 N2 Pd1 47.4(4) . . . . ?
C8 C7 N2 C5 57.1(4) . . . . ?
C8 C7 N2 C1 -65.2(3) . . . . ?
C8 C7 N2 Pd1 -178.3(2) . . . . ?
C2 C1 N2 C5 161.2(3) . . . . ?
C2 C1 N2 C7 -76.5(3) . . . . ?
C2 C1 N2 Pd1 37.5(3) . . . . ?
C1 C2 N3 C3 168.5(2) . . . . ?
C1 C2 N3 Pd1 45.4(3) . . . . ?
C4 C3 N3 C2 -171.3(2) . . . . ?
C4 C3 N3 Pd1 -47.9(3) . . . . ?
C10 C9 N4 C4 72.0(3) . . . . ?
C10 C9 N4 C11 -165.4(3) . . . . ?
C10 C9 N4 Pd1 -46.6(3) . . . . ?
C3 C4 N4 C9 -157.0(3) . . . . ?
C3 C4 N4 C11 80.2(3) . . . . ?
C3 C4 N4 Pd1 -33.1(3) . . . . ?
C12 C11 N4 C9 -56.3(4) . . . . ?
C12 C11 N4 C4 66.4(4) . . . . ?
C12 C11 N4 Pd1 179.6(3) . . . . ?
F3 C13 S1 O5 -179.0(2) . . . . ?
F2 C13 S1 O5 -59.4(3) . . . . ?
F1 C13 S1 O5 61.1(3) . . . . ?
F3 C13 S1 O3 59.9(3) . . . . ?
F2 C13 S1 O3 179.5(2) . . . . ?
F1 C13 S1 O3 -60.1(3) . . . . ?
F3 C13 S1 O4 -59.1(3) . . . . ?
F2 C13 S1 O4 60.5(3) . . . . ?
F1 C13 S1 O4 -179.0(2) . . . . ?

_refine_diff_density_max         0.589
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.086

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_VT_180K
_database_code_depnum_ccdc_archive 'CCDC 1564447'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3070(10)
_cell_length_b                   13.0321(14)
_cell_length_c                   16.893(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.340(11)
_cell_angle_gamma                90
_cell_volume                     2027.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2660
_cell_measurement_theta_min      3.8630
_cell_measurement_theta_max      29.1880

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.076
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.67284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            7201
_diffrn_reflns_av_unetI/netI     0.1137
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.356
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.348
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             3617
_reflns_number_gt                2461
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0966P)²+17.0016P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3617
_refine_ls_number_parameters     270
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0881
_refine_ls_wR_factor_ref         0.2445
_refine_ls_wR_factor_gt          0.2070
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.084
_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 0.2552(13) 0.4373(8) 0.4079(7) 0.035(2) Uani 1 1 d . U . . .
H1A H 0.1927 0.3814 0.3862 0.042 Uiso 1 1 calc R U . . .
H1B H 0.2509 0.4419 0.4648 0.042 Uiso 1 1 calc R U . . .
C2 C 0.4104(13) 0.4161(9) 0.3942(7) 0.037(2) Uani 1 1 d . U . . .
H2A H 0.4750 0.4691 0.4191 0.044 Uiso 1 1 calc R U . . .
H2B H 0.4429 0.3503 0.4171 0.044 Uiso 1 1 calc R U . . .
C3 C 0.5482(12) 0.4190(9) 0.2768(7) 0.033(2) Uani 1 1 d . U . . .
H3A H 0.5999 0.3547 0.2874 0.040 Uiso 1 1 calc R U . . .
H3B H 0.6082 0.4740 0.3022 0.040 Uiso 1 1 calc R U . . .
C4 C 0.5136(12) 0.4375(8) 0.1872(7) 0.0333(19) Uani 1 1 d . U . . .
H4A H 0.6031 0.4442 0.1645 0.040 Uiso 1 1 calc R U . . .
H4B H 0.4598 0.3796 0.1618 0.040 Uiso 1 1 calc R U . . .
C5 C 0.0423(12) 0.5381(9) 0.3581(7) 0.035(2) Uani 1 1 d . U . . .
H5A H 0.0103 0.6057 0.3391 0.042 Uiso 1 1 calc R U . . .
H5B H 0.0111 0.5282 0.4100 0.042 Uiso 1 1 calc R U . . .
C6 C -0.0323(15) 0.4573(11) 0.2998(9) 0.055(4) Uani 1 1 d . U . . .
H6A H 0.0192 0.4513 0.2548 0.083 Uiso 1 1 calc R U . . .
H6B H -0.1306 0.4780 0.2818 0.083 Uiso 1 1 calc R U . . .
H6C H -0.0322 0.3923 0.3266 0.083 Uiso 1 1 calc R U . . .
C7 C 0.2657(12) 0.6261(8) 0.4162(7) 0.033(2) Uani 1 1 d . U . . .
H7A H 0.2365 0.6875 0.3855 0.039 Uiso 1 1 calc R U . . .
H7B H 0.3707 0.6221 0.4218 0.039 Uiso 1 1 calc R U . . .
C8 C 0.2228(13) 0.6390(10) 0.4992(7) 0.042(3) Uani 1 1 d . U . . .
H8A H 0.1227 0.6592 0.4944 0.063 Uiso 1 1 calc R U . . .
H8B H 0.2825 0.6907 0.5279 0.063 Uiso 1 1 calc R U . . .
H8C H 0.2360 0.5751 0.5276 0.063 Uiso 1 1 calc R U . . .
C9 C 0.3457(13) 0.5322(8) 0.0883(7) 0.034(2) Uani 1 1 d . U . . .
H9A H 0.4152 0.5207 0.0516 0.041 Uiso 1 1 calc R U . . .
H9B H 0.3015 0.5988 0.0761 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2300(15) 0.4512(9) 0.0747(8) 0.047(3) Uani 1 1 d . U . . .
H10A H 0.1765 0.4588 0.0220 0.070 Uiso 1 1 calc R U . . .
H10B H 0.1652 0.4585 0.1137 0.070 Uiso 1 1 calc R U . . .
H10C H 0.2743 0.3846 0.0798 0.070 Uiso 1 1 calc R U . . .
C11 C 0.5151(12) 0.6275(8) 0.1844(7) 0.035(2) Uani 1 1 d . U . . .
H11A H 0.5671 0.6258 0.2385 0.042 Uiso 1 1 calc R U . . .
H11B H 0.4505 0.6863 0.1809 0.042 Uiso 1 1 calc R U . . .
C12 C 0.6272(14) 0.6456(10) 0.1264(8) 0.046(3) Uani 1 1 d . U . . .
H12A H 0.5788 0.6435 0.0722 0.069 Uiso 1 1 calc R U . . .
H12B H 0.7001 0.5930 0.1341 0.069 Uiso 1 1 calc R U . . .
H12C H 0.6720 0.7115 0.1369 0.069 Uiso 1 1 calc R U . . .
N2 N 0.2041(10) 0.5347(6) 0.3683(5) 0.0294(14) Uani 1 1 d . U . . .
N3 N 0.4100(10) 0.4155(7) 0.3074(5) 0.0314(16) Uani 1 1 d . U . . .
H3 H 0.3583 0.3537 0.2859 0.038 Uiso 1 1 calc R U . . .
N4 N 0.4249(10) 0.5338(6) 0.1721(6) 0.0312(14) Uani 1 1 d . U . . .
Pd1 Pd 0.29400(8) 0.53833(6) 0.26225(5) 0.0245(3) Uani 1 1 d D U . . .
N1 N 0.188(2) 0.6672(12) 0.2239(14) 0.026(4) Uani 0.367(19) 1 d D U P A 1
O1 O 0.234(2) 0.7480(11) 0.2491(14) 0.053(7) Uani 0.367(19) 1 d D U P A 1
O2 O 0.081(3) 0.6596(15) 0.175(2) 0.053(7) Uani 0.367(19) 1 d D U P A 1
N1A N 0.0722(16) 0.6842(9) 0.1740(12) 0.046(5) Uani 0.633(19) 1 d D U P A 2
O1A O 0.1935(14) 0.6750(10) 0.2227(10) 0.033(3) Uani 0.633(19) 1 d D U P A 2
O2A O 0.0196(13) 0.5947(9) 0.1547(9) 0.052(4) Uani 0.633(19) 1 d D U P A 2
C13 C 0.6108(12) 0.8038(9) 0.4070(7) 0.0370(13) Uani 1 1 d . U . . .
F1 F 0.6553(7) 0.8993(5) 0.4033(4) 0.0450(16) Uani 1 1 d . U . . .
F2 F 0.5571(8) 0.7922(5) 0.4755(4) 0.0491(16) Uani 1 1 d . U . . .
F3 F 0.4968(7) 0.7924(5) 0.3482(4) 0.0439(15) Uani 1 1 d . U . . .
O3 O 0.7923(9) 0.7372(6) 0.3189(5) 0.0433(18) Uani 1 1 d . U . . .
O4 O 0.6798(8) 0.6158(6) 0.3994(5) 0.0375(17) Uani 1 1 d . U . . .
O5 O 0.8597(9) 0.7356(6) 0.4640(5) 0.0460(18) Uani 1 1 d . U . . .
S1 S 0.7525(3) 0.7120(2) 0.39596(18) 0.0332(6) Uani 1 1 d . 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
C1 N2 1.481(14) . ?
C1 C2 1.521(15) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.467(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.455(13) . ?
C3 C4 1.520(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.504(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.491(14) . ?
C5 C6 1.536(17) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.505(14) . ?
C7 C8 1.522(15) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.498(15) . ?
C9 C10 1.502(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.479(14) . ?
C11 C12 1.550(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N2 Pd1 2.086(9) . ?
N3 Pd1 2.017(8) . ?
N3 H3 0.9800 . ?
N4 Pd1 2.085(8) . ?
Pd1 N1 2.007(14) . ?
Pd1 O1A 2.076(13) . ?
N1 O1 1.193(10) . ?
N1 O2 1.207(9) . ?
N1A O2A 1.289(9) . ?
N1A O1A 1.303(9) . ?
C13 F1 1.317(13) . ?
C13 F2 1.333(13) . ?
C13 F3 1.352(14) . ?
C13 S1 1.810(11) . ?
O3 S1 1.443(8) . ?
O4 S1 1.430(8) . ?
O5 S1 1.442(9) . ?

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
N2 C1 C2 109.7(9) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.7(10) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.7(9) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 109.5(9) . . ?
N4 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N4 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.1(9) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.8(9) . . ?
N2 C7 H7A 108.1 . . ?
C8 C7 H7A 108.1 . . ?
N2 C7 H7B 108.1 . . ?
C8 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.4(9) . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 117.2(9) . . ?
N4 C11 H11A 108.0 . . ?
C12 C11 H11A 108.0 . . ?
N4 C11 H11B 108.0 . . ?
C12 C11 H11B 108.0 . . ?
H11A C11 H11B 107.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 N2 C5 109.3(8) . . ?
C1 N2 C7 111.3(9) . . ?
C5 N2 C7 109.8(8) . . ?
C1 N2 Pd1 105.3(6) . . ?
C5 N2 Pd1 115.1(7) . . ?
C7 N2 Pd1 105.9(6) . . ?
C3 N3 C2 118.7(9) . . ?
C3 N3 Pd1 107.1(6) . . ?
C2 N3 Pd1 107.3(7) . . ?
C3 N3 H3 107.8 . . ?
C2 N3 H3 107.8 . . ?
Pd1 N3 H3 107.8 . . ?
C11 N4 C9 109.6(8) . . ?
C11 N4 C4 112.3(9) . . ?
C9 N4 C4 109.4(8) . . ?
C11 N4 Pd1 104.7(6) . . ?
C9 N4 Pd1 115.5(7) . . ?
C4 N4 Pd1 105.3(6) . . ?
N1 Pd1 N3 175.5(6) . . ?
N3 Pd1 O1A 173.4(4) . . ?
N1 Pd1 N4 95.7(8) . . ?
N3 Pd1 N4 85.2(3) . . ?
O1A Pd1 N4 94.2(5) . . ?
N1 Pd1 N2 93.3(8) . . ?
N3 Pd1 N2 85.2(3) . . ?
O1A Pd1 N2 94.5(5) . . ?
N4 Pd1 N2 167.7(4) . . ?
O1 N1 O2 122.5(13) . . ?
O1 N1 Pd1 119.2(11) . . ?
O2 N1 Pd1 118.2(11) . . ?
O2A N1A O1A 109.8(9) . . ?
N1A O1A Pd1 126.2(8) . . ?
F1 C13 F2 108.0(9) . . ?
F1 C13 F3 106.7(9) . . ?
F2 C13 F3 105.8(9) . . ?
F1 C13 S1 112.4(8) . . ?
F2 C13 S1 112.6(8) . . ?
F3 C13 S1 110.9(8) . . ?
O4 S1 O5 115.6(5) . . ?
O4 S1 O3 114.9(5) . . ?
O5 S1 O3 115.6(5) . . ?
O4 S1 C13 102.7(5) . . ?
O5 S1 C13 102.0(5) . . ?
O3 S1 C13 103.2(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
N2 C1 C2 N3 -56.5(12) . . . . ?
N3 C3 C4 N4 56.3(11) . . . . ?
C2 C1 N2 C5 161.4(9) . . . . ?
C2 C1 N2 C7 -77.2(11) . . . . ?
C2 C1 N2 Pd1 37.1(10) . . . . ?
C6 C5 N2 C1 -66.2(12) . . . . ?
C6 C5 N2 C7 171.4(10) . . . . ?
C6 C5 N2 Pd1 52.1(12) . . . . ?
C8 C7 N2 C1 -63.1(12) . . . . ?
C8 C7 N2 C5 58.0(12) . . . . ?
C8 C7 N2 Pd1 -177.1(8) . . . . ?
C4 C3 N3 C2 -169.7(9) . . . . ?
C4 C3 N3 Pd1 -48.1(10) . . . . ?
C1 C2 N3 C3 167.0(9) . . . . ?
C1 C2 N3 Pd1 45.6(10) . . . . ?
C12 C11 N4 C9 -56.3(12) . . . . ?
C12 C11 N4 C4 65.5(13) . . . . ?
C12 C11 N4 Pd1 179.2(9) . . . . ?
C10 C9 N4 C11 -168.8(9) . . . . ?
C10 C9 N4 C4 67.7(11) . . . . ?
C10 C9 N4 Pd1 -50.9(11) . . . . ?
C3 C4 N4 C11 78.8(11) . . . . ?
C3 C4 N4 C9 -159.3(9) . . . . ?
C3 C4 N4 Pd1 -34.6(10) . . . . ?
O2A N1A O1A Pd1 1.6(17) . . . . ?
F1 C13 S1 O4 -178.3(8) . . . . ?
F2 C13 S1 O4 59.4(9) . . . . ?
F3 C13 S1 O4 -58.9(9) . . . . ?
F1 C13 S1 O5 61.7(10) . . . . ?
F2 C13 S1 O5 -60.6(9) . . . . ?
F3 C13 S1 O5 -178.9(8) . . . . ?
F1 C13 S1 O3 -58.5(10) . . . . ?
F2 C13 S1 O3 179.2(8) . . . . ?
F3 C13 S1 O3 60.8(9) . . . . ?

_refine_diff_density_max         3.066
_refine_diff_density_min         -3.627
_refine_diff_density_rms         0.212

####################################################################### 
# 
# 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_Pt_VT_240K
_database_code_depnum_ccdc_archive 'CCDC 1564476'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_Pt_VT_240K          
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: The generally lower quality of diffraction data at 240 K is attributed to the observation that the photo-excited state in this material is known to have been dynamically decaying during this experiment. This is reflected in the intensity statistics, with a significantly reduced I/sigma level and poorer R-indicies than for other structures in this study.
;
# Added during the CSD deposition process: Tuesday 25 July 2017 11:25 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3167(8)
_cell_length_b                   13.0913(11)
_cell_length_c                   17.0815(16)
_cell_angle_alpha                90
_cell_angle_beta                 97.385(9)
_cell_angle_gamma                90
_cell_volume                     2066.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8345
_cell_measurement_theta_min      3.8860
_cell_measurement_theta_max      29.8100

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -5 0.1067
0 3 5 0.1696
3 5 -2 0.1520
3 -5 -2 0.1832
5 1 -4 0.0508
0 -1 -1 0.1437
1 0 5 0.1033
1 -5 3 0.2517
1 1 5 0.1103
-1 5 1 0.2318
5 0 -4 0.0512
-5 0 4 0.0348
_exptl_absorpt_coefficient_mu    6.949
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            22058
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_av_R_equivalents  0.1281
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.337
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4212
_reflns_number_gt                3235
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0348P)²+14.9547P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4212
_refine_ls_number_parameters     243
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1256
_refine_ls_wR_factor_gt          0.1101
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.059
_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 -0.0302(13) 0.5565(7) 0.8073(7) 0.0413(19) Uani 1 1 d . U . . .
H1A H 0.0207 0.6138 0.8341 0.050 Uiso 1 1 calc R U . . .
H1B H -0.1213 0.5482 0.8284 0.050 Uiso 1 1 calc R U . . .
C2 C -0.0596(11) 0.5787(8) 0.7204(6) 0.0375(18) Uani 1 1 d . U . . .
H2A H -0.1218 0.5267 0.6936 0.045 Uiso 1 1 calc R U . . .
H2B H -0.1059 0.6448 0.7112 0.045 Uiso 1 1 calc R U . . .
C3 C 0.0864(12) 0.5832(8) 0.6058(6) 0.0387(18) Uani 1 1 d . U . . .
H3A H 0.0556 0.6501 0.5858 0.046 Uiso 1 1 calc R U . . .
H3B H 0.0222 0.5322 0.5792 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2378(12) 0.5633(8) 0.5926(7) 0.0407(19) Uani 1 1 d . U . . .
H4A H 0.2991 0.6191 0.6141 0.049 Uiso 1 1 calc R U . . .
H4B H 0.2437 0.5591 0.5365 0.049 Uiso 1 1 calc R U . . .
C5 C -0.0331(13) 0.3675(8) 0.8104(7) 0.046(2) Uani 1 1 d . U . . .
H5A H 0.0298 0.3083 0.8124 0.055 Uiso 1 1 calc R U . . .
H5B H -0.0873 0.3702 0.7580 0.055 Uiso 1 1 calc R U . . .
C6 C -0.1396(17) 0.3531(11) 0.8706(9) 0.075(4) Uani 1 1 d . U . . .
H6A H -0.2068 0.2997 0.8530 0.113 Uiso 1 1 calc R U . . .
H6B H -0.1914 0.4156 0.8757 0.113 Uiso 1 1 calc R U . . .
H6C H -0.0874 0.3348 0.9208 0.113 Uiso 1 1 calc R U . . .
C7 C 0.1372(14) 0.4632(8) 0.9062(7) 0.048(2) Uani 1 1 d . U . . .
H7A H 0.1793 0.3964 0.9185 0.057 Uiso 1 1 calc R U . . .
H7B H 0.0674 0.4761 0.9425 0.057 Uiso 1 1 calc R U . . .
C8 C 0.2562(16) 0.5431(9) 0.9191(9) 0.063(3) Uani 1 1 d . U . . .
H8A H 0.3361 0.5226 0.8925 0.095 Uiso 1 1 calc R U . . .
H8B H 0.2881 0.5497 0.9746 0.095 Uiso 1 1 calc R U . . .
H8C H 0.2195 0.6076 0.8985 0.095 Uiso 1 1 calc R U . . .
C9 C 0.2320(11) 0.3767(8) 0.5801(6) 0.0387(19) Uani 1 1 d . U . . .
H9A H 0.2543 0.3135 0.6087 0.046 Uiso 1 1 calc R U . . .
H9B H 0.1275 0.3831 0.5714 0.046 Uiso 1 1 calc R U . . .
C10 C 0.2845(13) 0.3665(10) 0.5008(7) 0.057(3) Uani 1 1 d . U . . .
H10A H 0.2754 0.4311 0.4739 0.085 Uiso 1 1 calc R U . . .
H10B H 0.2275 0.3162 0.4700 0.085 Uiso 1 1 calc R U . . .
H10C H 0.3842 0.3458 0.5078 0.085 Uiso 1 1 calc R U . . .
C11 C 0.4512(12) 0.4603(9) 0.6413(7) 0.044(2) Uani 1 1 d . U . . .
H11A H 0.4831 0.4761 0.5908 0.052 Uiso 1 1 calc R U . . .
H11B H 0.4829 0.3914 0.6555 0.052 Uiso 1 1 calc R U . . .
C12 C 0.5240(15) 0.5345(12) 0.7035(9) 0.074(4) Uani 1 1 d . U . . .
H12A H 0.4989 0.6033 0.6880 0.111 Uiso 1 1 calc R U . . .
H12B H 0.6272 0.5263 0.7080 0.111 Uiso 1 1 calc R U . . .
H12C H 0.4917 0.5203 0.7535 0.111 Uiso 1 1 calc R U . . .
N2 N 0.0588(10) 0.4615(6) 0.8226(5) 0.0380(14) Uani 1 1 d . U . . .
N3 N 0.0841(9) 0.5782(6) 0.6921(5) 0.0320(14) Uani 1 1 d . U . . .
H3 H 0.1362 0.6385 0.7149 0.038 Uiso 1 1 calc R U . . .
N4 N 0.2906(9) 0.4636(6) 0.6324(5) 0.0324(12) Uani 1 1 d . U . . .
Pt1 Pt 0.19514(5) 0.45739(3) 0.73451(2) 0.02963(14) Uani 1 1 d . U . . .
N1 N 0.3009(9) 0.3292(6) 0.7733(5) 0.0581(15) Uani 0.659(12) 1 d D U P A 1
O1 O 0.2671(13) 0.2509(8) 0.7423(7) 0.0581(15) Uani 0.659(12) 1 d D U P A 1
O2 O 0.3991(13) 0.3363(8) 0.8271(7) 0.0581(15) Uani 0.659(12) 1 d D U P A 1
N1A N 0.4245(17) 0.3107(13) 0.8169(12) 0.0581(15) Uani 0.341(12) 1 d D U P A 2
O1A O 0.3009(9) 0.3292(6) 0.7733(5) 0.0581(15) Uani 0.341(12) 1 d D U P A 2
O2A O 0.4773(19) 0.3996(14) 0.8400(13) 0.0581(15) Uani 0.341(12) 1 d D U P A 2
C13 C 0.6113(13) 0.6915(9) 0.9099(7) 0.0495(14) Uani 1 1 d . U . . .
F1 F 0.6578(8) 0.5962(5) 0.9068(5) 0.0625(17) Uani 1 1 d . U . . .
F2 F 0.5579(9) 0.7037(5) 0.9775(5) 0.0672(18) Uani 1 1 d . U . . .
F3 F 0.5016(8) 0.7031(6) 0.8531(5) 0.0652(17) Uani 1 1 d . U . . .
O3 O 0.8584(9) 0.7608(7) 0.9643(6) 0.065(2) Uani 1 1 d . U . . .
O4 O 0.6809(9) 0.8791(5) 0.9026(5) 0.0512(18) Uani 1 1 d . U . . .
O5 O 0.7922(9) 0.7593(6) 0.8214(5) 0.0575(18) Uani 1 1 d . U . . .
S1 S 0.7537(3) 0.7833(2) 0.89874(18) 0.0445(6) Uani 1 1 d . 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
C1 N2 1.499(13) . ?
C1 C2 1.502(15) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.481(12) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.479(13) . ?
C3 C4 1.480(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.523(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.498(13) . ?
C5 C6 1.528(15) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.518(15) . ?
C7 C8 1.520(17) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.504(15) . ?
C9 N4 1.506(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.485(13) . ?
C11 C12 1.532(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N2 Pt1 2.091(8) . ?
N3 Pt1 1.976(7) . ?
N3 H3 0.9800 . ?
N4 Pt1 2.058(8) . ?
Pt1 O1A 2.014(8) . ?
Pt1 N1 2.014(8) . ?
N1 O1 1.178(8) . ?
N1 O2 1.215(8) . ?
N1A O2A 1.304(10) . ?
N1A O1A 1.312(10) . ?
C13 F2 1.324(13) . ?
C13 F1 1.325(13) . ?
C13 F3 1.325(14) . ?
C13 S1 1.817(12) . ?
O3 S1 1.418(9) . ?
O4 S1 1.432(8) . ?
O5 S1 1.447(9) . ?

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
N2 C1 C2 111.1(8) . . ?
N2 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N2 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 105.3(9) . . ?
N3 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
N3 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
N3 C3 C4 106.2(9) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 110.0(8) . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
N4 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.6(9) . . ?
N2 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
N2 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 113.6(9) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N4 117.8(9) . . ?
C10 C9 H9A 107.8 . . ?
N4 C9 H9A 107.8 . . ?
C10 C9 H9B 107.8 . . ?
N4 C9 H9B 107.8 . . ?
H9A C9 H9B 107.2 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 113.7(9) . . ?
N4 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N4 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 111.3(9) . . ?
C5 N2 C7 109.9(8) . . ?
C1 N2 C7 110.0(8) . . ?
C5 N2 Pt1 105.5(6) . . ?
C1 N2 Pt1 105.6(6) . . ?
C7 N2 Pt1 114.4(7) . . ?
C3 N3 C2 117.0(8) . . ?
C3 N3 Pt1 109.1(6) . . ?
C2 N3 Pt1 109.7(6) . . ?
C3 N3 H3 106.8 . . ?
C2 N3 H3 106.8 . . ?
Pt1 N3 H3 106.8 . . ?
C11 N4 C9 108.8(7) . . ?
C11 N4 C4 109.5(8) . . ?
C9 N4 C4 108.1(8) . . ?
C11 N4 Pt1 116.9(7) . . ?
C9 N4 Pt1 108.1(6) . . ?
C4 N4 Pt1 105.2(6) . . ?
N3 Pt1 O1A 176.7(3) . . ?
N3 Pt1 N1 176.7(3) . . ?
N3 Pt1 N4 85.5(3) . . ?
O1A Pt1 N4 93.7(3) . . ?
N1 Pt1 N4 93.7(3) . . ?
N3 Pt1 N2 84.5(3) . . ?
O1A Pt1 N2 95.8(3) . . ?
N1 Pt1 N2 95.8(3) . . ?
N4 Pt1 N2 167.7(4) . . ?
O1 N1 O2 122.6(9) . . ?
O1 N1 Pt1 119.1(7) . . ?
O2 N1 Pt1 118.3(7) . . ?
O2A N1A O1A 106.1(10) . . ?
N1A O1A Pt1 134.2(8) . . ?
F2 C13 F1 108.0(10) . . ?
F2 C13 F3 106.5(10) . . ?
F1 C13 F3 107.7(10) . . ?
F2 C13 S1 111.9(8) . . ?
F1 C13 S1 111.8(8) . . ?
F3 C13 S1 110.6(8) . . ?
O3 S1 O4 115.3(5) . . ?
O3 S1 O5 116.7(6) . . ?
O4 S1 O5 114.0(5) . . ?
O3 S1 C13 102.6(6) . . ?
O4 S1 C13 102.6(5) . . ?
O5 S1 C13 102.9(5) . . ?

_refine_diff_density_max         1.885
_refine_diff_density_min         -1.786
_refine_diff_density_rms         0.219

####################################################################### 
# 
# 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_VT_210K
_database_code_depnum_ccdc_archive 'CCDC 1564446'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) 
trifluoromethanesulfonate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2551(4)
_cell_length_b                   13.1357(5)
_cell_length_c                   17.1243(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.291(5)
_cell_angle_gamma                90
_cell_volume                     2069.30(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    272(2)
_cell_measurement_reflns_used    3015
_cell_measurement_theta_min      3.7720
_cell_measurement_theta_max      29.4280

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.054
_shelx_estimated_absorpt_T_min   0.648
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      272(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9035
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.325
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4221
_reflns_number_gt                3352
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0237P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4221
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0664
_refine_ls_wR_factor_gt          0.0602
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 0.2583(3) 0.4383(2) 0.40746(19) 0.0352(8) Uani 1 1 d . . . . .
H1A H 0.1971 0.3840 0.3841 0.042 Uiso 1 1 calc R U . . .
H1B H 0.2484 0.4403 0.4632 0.042 Uiso 1 1 calc R U . . .
C2 C 0.4141(3) 0.4172(2) 0.39558(19) 0.0330(7) Uani 1 1 d . . . . .
H2A H 0.4779 0.4678 0.4224 0.040 Uiso 1 1 calc R U . . .
H2B H 0.4432 0.3504 0.4156 0.040 Uiso 1 1 calc R U . . .
C3 C 0.5655(3) 0.4249(2) 0.2817(2) 0.0331(8) Uani 1 1 d . . . . .
H3A H 0.6149 0.3603 0.2914 0.040 Uiso 1 1 calc R U . . .
H3B H 0.6246 0.4782 0.3082 0.040 Uiso 1 1 calc R U . . .
C4 C 0.5393(3) 0.4459(2) 0.19527(19) 0.0346(8) Uani 1 1 d . . . . .
H4A H 0.4893 0.3885 0.1689 0.041 Uiso 1 1 calc R U . . .
H4B H 0.6317 0.4542 0.1742 0.041 Uiso 1 1 calc R U . . .
C5 C 0.0471(3) 0.5429(3) 0.3581(2) 0.0430(9) Uani 1 1 d . . . . .
H5A H 0.0185 0.6123 0.3448 0.052 Uiso 1 1 calc R U . . .
H5B H 0.0087 0.5260 0.4070 0.052 Uiso 1 1 calc R U . . .
C6 C -0.0203(4) 0.4731(3) 0.2948(2) 0.0605(12) Uani 1 1 d . . . . .
H6A H 0.0170 0.4891 0.2461 0.091 Uiso 1 1 calc R U . . .
H6B H -0.1239 0.4819 0.2889 0.091 Uiso 1 1 calc R U . . .
H6C H 0.0029 0.4038 0.3088 0.091 Uiso 1 1 calc R U . . .
C7 C 0.2691(3) 0.6247(2) 0.42092(18) 0.0346(8) Uani 1 1 d . . . . .
H7A H 0.2458 0.6875 0.3925 0.042 Uiso 1 1 calc R U . . .
H7B H 0.3742 0.6188 0.4284 0.042 Uiso 1 1 calc R U . . .
C8 C 0.2144(4) 0.6332(3) 0.5015(2) 0.0497(10) Uani 1 1 d . . . . .
H8A H 0.1114 0.6452 0.4951 0.075 Uiso 1 1 calc R U . . .
H8B H 0.2626 0.6888 0.5300 0.075 Uiso 1 1 calc R U . . .
H8C H 0.2347 0.5711 0.5301 0.075 Uiso 1 1 calc R U . . .
C9 C 0.3737(4) 0.5388(2) 0.09782(19) 0.0401(8) Uani 1 1 d . . . . .
H9A H 0.4440 0.5222 0.0617 0.048 Uiso 1 1 calc R U . . .
H9B H 0.3360 0.6063 0.0845 0.048 Uiso 1 1 calc R U . . .
C10 C 0.2500(4) 0.4631(3) 0.0867(2) 0.0530(10) Uani 1 1 d . . . . .
H10A H 0.2067 0.4650 0.0332 0.080 Uiso 1 1 calc R U . . .
H10B H 0.1783 0.4803 0.1210 0.080 Uiso 1 1 calc R U . . .
H10C H 0.2865 0.3959 0.0990 0.080 Uiso 1 1 calc R U . . .
C11 C 0.5435(3) 0.6336(2) 0.1924(2) 0.0380(8) Uani 1 1 d . . . . .
H11A H 0.5935 0.6308 0.2452 0.046 Uiso 1 1 calc R U . . .
H11B H 0.4814 0.6932 0.1893 0.046 Uiso 1 1 calc R U . . .
C12 C 0.6568(4) 0.6472(3) 0.1348(3) 0.0640(12) Uani 1 1 d . . . . .
H12A H 0.6086 0.6579 0.0829 0.096 Uiso 1 1 calc R U . . .
H12B H 0.7162 0.5873 0.1352 0.096 Uiso 1 1 calc R U . . .
H12C H 0.7167 0.7050 0.1501 0.096 Uiso 1 1 calc R U . . .
N1 N 0.2017(3) 0.67043(19) 0.22669(17) 0.0344(6) Uani 1 1 d . . . . .
N2 N 0.2097(2) 0.53761(17) 0.37081(15) 0.0271(6) Uani 1 1 d . . . . .
N3 N 0.4202(2) 0.42212(16) 0.31007(14) 0.0232(5) Uani 1 1 d . . . . .
H3 H 0.3694 0.3621 0.2868 0.028 Uiso 1 1 calc R U . . .
N4 N 0.4492(3) 0.54086(17) 0.17957(15) 0.0277(6) Uani 1 1 d . . . . .
O1 O 0.2385(3) 0.75291(19) 0.25490(18) 0.0707(9) Uani 1 1 d . . . . .
O2 O 0.0991(3) 0.6688(2) 0.17606(19) 0.0818(10) Uani 1 1 d . . . . .
Pd1 Pd 0.31038(2) 0.54498(2) 0.26778(2) 0.02193(8) Uani 1 1 d . . . . .
C13 C 0.6106(4) 0.8125(2) 0.4134(2) 0.0391(8) Uani 1 1 d . . . . .
F1 F 0.6605(2) 0.90709(13) 0.41147(14) 0.0573(6) Uani 1 1 d . . . . .
F2 F 0.5557(2) 0.80136(15) 0.48121(13) 0.0628(6) Uani 1 1 d . . . . .
F3 F 0.5018(2) 0.80408(16) 0.35679(14) 0.0633(6) Uani 1 1 d . . . . .
O3 O 0.7946(3) 0.74344(17) 0.32615(15) 0.0520(7) Uani 1 1 d . . . . .
O4 O 0.6747(2) 0.62408(15) 0.40468(14) 0.0433(6) Uani 1 1 d . . . . .
O5 O 0.8564(3) 0.73840(19) 0.46738(17) 0.0605(7) Uani 1 1 d . . . . .
S1 S 0.75125(9) 0.71926(6) 0.40164(5) 0.0354(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.495(4) . ?
C1 C2 1.503(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.473(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.479(3) . ?
C3 C4 1.499(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.508(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.499(4) . ?
C5 C6 1.503(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.498(4) . ?
C7 C8 1.525(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.495(4) . ?
C9 C10 1.513(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.500(4) . ?
C11 C12 1.526(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N1 O2 1.214(3) . ?
N1 O1 1.220(4) . ?
N1 Pd1 2.017(2) . ?
N2 Pd1 2.086(2) . ?
N3 Pd1 2.000(2) . ?
N3 H3 0.9800 . ?
N4 Pd1 2.088(2) . ?
C13 F3 1.324(4) . ?
C13 F2 1.326(4) . ?
C13 F1 1.328(4) . ?
C13 S1 1.814(3) . ?
O3 S1 1.431(2) . ?
O4 S1 1.441(2) . ?
O5 S1 1.428(3) . ?

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
N2 C1 C2 110.7(2) . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.6(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.8 . . ?
N3 C3 C4 105.9(2) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 110.7(2) . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 114.0(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 115.9(3) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.5(3) . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 115.5(3) . . ?
N4 C11 H11A 108.4 . . ?
C12 C11 H11A 108.4 . . ?
N4 C11 H11B 108.4 . . ?
C12 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 N1 O1 117.5(3) . . ?
O2 N1 Pd1 123.8(2) . . ?
O1 N1 Pd1 118.7(2) . . ?
C1 N2 C7 110.6(2) . . ?
C1 N2 C5 110.6(2) . . ?
C7 N2 C5 110.3(2) . . ?
C1 N2 Pd1 104.70(16) . . ?
C7 N2 Pd1 106.20(17) . . ?
C5 N2 Pd1 114.2(2) . . ?
C2 N3 C3 117.6(2) . . ?
C2 N3 Pd1 108.77(17) . . ?
C3 N3 Pd1 107.79(17) . . ?
C2 N3 H3 107.4 . . ?
C3 N3 H3 107.4 . . ?
Pd1 N3 H3 107.4 . . ?
C9 N4 C11 110.9(2) . . ?
C9 N4 C4 110.2(2) . . ?
C11 N4 C4 110.1(2) . . ?
C9 N4 Pd1 114.59(18) . . ?
C11 N4 Pd1 105.51(17) . . ?
C4 N4 Pd1 105.33(17) . . ?
N3 Pd1 N1 178.94(11) . . ?
N3 Pd1 N2 85.00(9) . . ?
N1 Pd1 N2 94.65(10) . . ?
N3 Pd1 N4 84.97(9) . . ?
N1 Pd1 N4 95.26(10) . . ?
N2 Pd1 N4 167.93(9) . . ?
F3 C13 F2 107.3(3) . . ?
F3 C13 F1 107.4(3) . . ?
F2 C13 F1 107.0(3) . . ?
F3 C13 S1 111.1(2) . . ?
F2 C13 S1 111.8(2) . . ?
F1 C13 S1 111.9(2) . . ?
O5 S1 O3 116.02(16) . . ?
O5 S1 O4 114.83(16) . . ?
O3 S1 O4 114.39(15) . . ?
O5 S1 C13 103.25(16) . . ?
O3 S1 C13 103.06(15) . . ?
O4 S1 C13 102.72(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 -55.7(3) . . . . ?
N3 C3 C4 N4 54.4(3) . . . . ?
C2 C1 N2 C7 -76.6(3) . . . . ?
C2 C1 N2 C5 160.9(3) . . . . ?
C2 C1 N2 Pd1 37.4(3) . . . . ?
C8 C7 N2 C1 -65.1(3) . . . . ?
C8 C7 N2 C5 57.6(4) . . . . ?
C8 C7 N2 Pd1 -178.1(2) . . . . ?
C6 C5 N2 C1 -70.2(4) . . . . ?
C6 C5 N2 C7 167.2(3) . . . . ?
C6 C5 N2 Pd1 47.6(4) . . . . ?
C1 C2 N3 C3 167.9(2) . . . . ?
C1 C2 N3 Pd1 45.1(3) . . . . ?
C4 C3 N3 C2 -171.5(2) . . . . ?
C4 C3 N3 Pd1 -48.2(3) . . . . ?
C10 C9 N4 C11 -165.6(3) . . . . ?
C10 C9 N4 C4 72.2(3) . . . . ?
C10 C9 N4 Pd1 -46.4(3) . . . . ?
C12 C11 N4 C9 -55.9(4) . . . . ?
C12 C11 N4 C4 66.2(4) . . . . ?
C12 C11 N4 Pd1 179.4(3) . . . . ?
C3 C4 N4 C9 -156.9(2) . . . . ?
C3 C4 N4 C11 80.5(3) . . . . ?
C3 C4 N4 Pd1 -32.9(3) . . . . ?
F3 C13 S1 O5 -179.1(2) . . . . ?
F2 C13 S1 O5 -59.2(3) . . . . ?
F1 C13 S1 O5 60.8(3) . . . . ?
F3 C13 S1 O3 59.7(3) . . . . ?
F2 C13 S1 O3 179.6(2) . . . . ?
F1 C13 S1 O3 -60.3(3) . . . . ?
F3 C13 S1 O4 -59.4(3) . . . . ?
F2 C13 S1 O4 60.5(3) . . . . ?
F1 C13 S1 O4 -179.5(2) . . . . ?

_refine_diff_density_max         0.466
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.082

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_VT_300K
_database_code_depnum_ccdc_archive 'CCDC 1564448'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) 
trifluoromethanesulfonate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3062(5)
_cell_length_b                   13.1239(6)
_cell_length_c                   17.3489(12)
_cell_angle_alpha                90
_cell_angle_beta                 95.366(6)
_cell_angle_gamma                90
_cell_volume                     2109.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    2600
_cell_measurement_theta_min      3.8190
_cell_measurement_theta_max      29.1880

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.034
_shelx_estimated_absorpt_T_min   0.653
_shelx_estimated_absorpt_T_max   0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9245
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.321
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.000
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4310
_reflns_number_gt                3196
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0253P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4310
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0754
_refine_ls_wR_factor_gt          0.0666
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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 0.2584(4) 0.4387(3) 0.4068(2) 0.0513(10) Uani 1 1 d . . . . .
H1A H 0.2474 0.4409 0.4618 0.062 Uiso 1 1 calc R U . . .
H1B H 0.1987 0.3838 0.3841 0.062 Uiso 1 1 calc R U . . .
C2 C 0.4129(4) 0.4189(3) 0.3946(2) 0.0499(10) Uani 1 1 d . . . . .
H2A H 0.4748 0.4702 0.4207 0.060 Uiso 1 1 calc R U . . .
H2B H 0.4425 0.3524 0.4147 0.060 Uiso 1 1 calc R U . . .
C3 C 0.5664(4) 0.4262(3) 0.2824(2) 0.0490(10) Uani 1 1 d . . . . .
H3A H 0.6152 0.3614 0.2916 0.059 Uiso 1 1 calc R U . . .
H3B H 0.6245 0.4793 0.3088 0.059 Uiso 1 1 calc R U . . .
C4 C 0.5429(4) 0.4479(3) 0.1973(2) 0.0541(11) Uani 1 1 d . . . . .
H4A H 0.6355 0.4563 0.1767 0.065 Uiso 1 1 calc R U . . .
H4B H 0.4940 0.3905 0.1712 0.065 Uiso 1 1 calc R U . . .
C5 C 0.0492(4) 0.5418(3) 0.3582(3) 0.0629(12) Uani 1 1 d . . . . .
H5A H 0.0197 0.6110 0.3450 0.075 Uiso 1 1 calc R U . . .
H5B H 0.0106 0.5246 0.4066 0.075 Uiso 1 1 calc R U . . .
C6 C -0.0158(4) 0.4715(4) 0.2962(3) 0.0860(16) Uani 1 1 d . . . . .
H6A H 0.0218 0.4877 0.2480 0.129 Uiso 1 1 calc R U . . .
H6B H -0.1188 0.4796 0.2908 0.129 Uiso 1 1 calc R U . . .
H6C H 0.0079 0.4023 0.3101 0.129 Uiso 1 1 calc R U . . .
C7 C 0.2676(4) 0.6256(3) 0.4201(2) 0.0520(10) Uani 1 1 d . . . . .
H7A H 0.2444 0.6887 0.3924 0.062 Uiso 1 1 calc R U . . .
H7B H 0.3720 0.6201 0.4269 0.062 Uiso 1 1 calc R U . . .
C8 C 0.2123(5) 0.6333(4) 0.4996(3) 0.0752(14) Uani 1 1 d . . . . .
H8A H 0.1096 0.6428 0.4938 0.113 Uiso 1 1 calc R U . . .
H8B H 0.2572 0.6902 0.5270 0.113 Uiso 1 1 calc R U . . .
H8C H 0.2352 0.5717 0.5280 0.113 Uiso 1 1 calc R U . . .
C9 C 0.3820(5) 0.5405(3) 0.1014(2) 0.0631(12) Uani 1 1 d . . . . .
H9A H 0.4535 0.5253 0.0658 0.076 Uiso 1 1 calc R U . . .
H9B H 0.3435 0.6078 0.0887 0.076 Uiso 1 1 calc R U . . .
C10 C 0.2606(5) 0.4633(3) 0.0895(3) 0.0828(15) Uani 1 1 d . . . . .
H10A H 0.2193 0.4658 0.0368 0.124 Uiso 1 1 calc R U . . .
H10B H 0.1878 0.4789 0.1234 0.124 Uiso 1 1 calc R U . . .
H10C H 0.2981 0.3962 0.1009 0.124 Uiso 1 1 calc R U . . .
C11 C 0.5476(4) 0.6352(3) 0.1942(2) 0.0591(11) Uani 1 1 d . . . . .
H11A H 0.5939 0.6333 0.2467 0.071 Uiso 1 1 calc R U . . .
H11B H 0.4855 0.6947 0.1902 0.071 Uiso 1 1 calc R U . . .
C12 C 0.6636(6) 0.6492(4) 0.1394(3) 0.0980(19) Uani 1 1 d . . . . .
H12A H 0.6193 0.6580 0.0876 0.147 Uiso 1 1 calc R U . . .
H12B H 0.7247 0.5901 0.1414 0.147 Uiso 1 1 calc R U . . .
H12C H 0.7203 0.7082 0.1544 0.147 Uiso 1 1 calc R U . . .
N1 N 0.2064(4) 0.6722(2) 0.2286(2) 0.0505(8) Uani 1 1 d . . . . .
N2 N 0.2096(3) 0.5382(2) 0.37009(17) 0.0396(7) Uani 1 1 d . . . . .
N3 N 0.4213(3) 0.42321(19) 0.31019(17) 0.0347(7) Uani 1 1 d . . . . .
H3 H 0.3716 0.3630 0.2874 0.042 Uiso 1 1 calc R U . . .
N4 N 0.4544(3) 0.5422(2) 0.18198(17) 0.0423(7) Uani 1 1 d . . . . .
O1 O 0.2392(4) 0.7539(2) 0.2553(2) 0.0985(13) Uani 1 1 d . . . . .
O2 O 0.1040(5) 0.6695(3) 0.1796(2) 0.1206(15) Uani 1 1 d . . . . .
Pd1 Pd 0.31282(3) 0.54619(2) 0.26876(2) 0.03292(10) Uani 1 1 d . . . . .
C13 C 0.6117(5) 0.8143(3) 0.4161(3) 0.0597(11) Uani 1 1 d . . . . .
F1 F 0.6607(3) 0.90811(17) 0.41410(18) 0.0901(9) Uani 1 1 d . . . . .
F2 F 0.5547(3) 0.8030(2) 0.48192(18) 0.0998(10) Uani 1 1 d . . . . .
F3 F 0.5040(3) 0.8063(2) 0.3609(2) 0.1026(10) Uani 1 1 d . . . . .
O3 O 0.7933(3) 0.7439(2) 0.32883(19) 0.0810(10) Uani 1 1 d . . . . .
O4 O 0.6731(3) 0.62593(19) 0.40676(17) 0.0675(8) Uani 1 1 d . . . . .
O5 O 0.8527(3) 0.7390(3) 0.4675(2) 0.0963(11) Uani 1 1 d . . . . .
S1 S 0.74961(11) 0.72046(8) 0.40361(7) 0.0543(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.495(5) . ?
C1 N2 1.503(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.476(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.476(4) . ?
C3 C4 1.499(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.497(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.489(4) . ?
C5 C6 1.501(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.508(4) . ?
C7 C8 1.520(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.495(5) . ?
C9 C10 1.517(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.500(4) . ?
C11 C12 1.516(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N1 O1 1.197(4) . ?
N1 O2 1.218(4) . ?
N1 Pd1 2.017(3) . ?
N2 Pd1 2.083(3) . ?
N3 Pd1 2.002(2) . ?
N3 H3 0.9800 . ?
N4 Pd1 2.092(3) . ?
C13 F2 1.312(5) . ?
C13 F1 1.315(4) . ?
C13 F3 1.324(5) . ?
C13 S1 1.806(4) . ?
O3 S1 1.429(3) . ?
O4 S1 1.434(3) . ?
O5 S1 1.417(3) . ?

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 N2 110.4(3) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.9(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.8(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 111.1(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 114.3(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.0(3) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.6(3) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.5(3) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 N1 O2 116.8(3) . . ?
O1 N1 Pd1 120.1(3) . . ?
O2 N1 Pd1 123.0(3) . . ?
C5 N2 C1 110.2(3) . . ?
C5 N2 C7 110.8(3) . . ?
C1 N2 C7 109.9(3) . . ?
C5 N2 Pd1 114.7(2) . . ?
C1 N2 Pd1 104.85(19) . . ?
C7 N2 Pd1 106.2(2) . . ?
C3 N3 C2 117.4(3) . . ?
C3 N3 Pd1 107.9(2) . . ?
C2 N3 Pd1 108.4(2) . . ?
C3 N3 H3 107.6 . . ?
C2 N3 H3 107.6 . . ?
Pd1 N3 H3 107.6 . . ?
C9 N4 C4 110.3(3) . . ?
C9 N4 C11 110.4(3) . . ?
C4 N4 C11 110.3(3) . . ?
C9 N4 Pd1 114.5(2) . . ?
C4 N4 Pd1 105.4(2) . . ?
C11 N4 Pd1 105.8(2) . . ?
N3 Pd1 N1 178.69(14) . . ?
N3 Pd1 N2 85.02(11) . . ?
N1 Pd1 N2 94.72(12) . . ?
N3 Pd1 N4 84.71(11) . . ?
N1 Pd1 N4 95.40(12) . . ?
N2 Pd1 N4 167.73(11) . . ?
F2 C13 F1 107.3(4) . . ?
F2 C13 F3 106.2(4) . . ?
F1 C13 F3 107.2(4) . . ?
F2 C13 S1 112.2(3) . . ?
F1 C13 S1 112.6(3) . . ?
F3 C13 S1 111.0(3) . . ?
O5 S1 O3 116.3(2) . . ?
O5 S1 O4 114.9(2) . . ?
O3 S1 O4 113.89(19) . . ?
O5 S1 C13 103.0(2) . . ?
O3 S1 C13 103.2(2) . . ?
O4 S1 C13 102.97(18) . . ?

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
N2 C1 C2 N3 -55.8(4) . . . . ?
N3 C3 C4 N4 54.4(4) . . . . ?
C6 C5 N2 C1 -70.4(4) . . . . ?
C6 C5 N2 C7 167.7(4) . . . . ?
C6 C5 N2 Pd1 47.6(4) . . . . ?
C2 C1 N2 C5 160.8(3) . . . . ?
C2 C1 N2 C7 -76.8(4) . . . . ?
C2 C1 N2 Pd1 36.9(3) . . . . ?
C8 C7 N2 C5 57.4(4) . . . . ?
C8 C7 N2 C1 -64.7(4) . . . . ?
C8 C7 N2 Pd1 -177.5(3) . . . . ?
C4 C3 N3 C2 -170.8(3) . . . . ?
C4 C3 N3 Pd1 -48.0(3) . . . . ?
C1 C2 N3 C3 168.4(3) . . . . ?
C1 C2 N3 Pd1 45.8(3) . . . . ?
C10 C9 N4 C4 71.1(4) . . . . ?
C10 C9 N4 C11 -166.7(3) . . . . ?
C10 C9 N4 Pd1 -47.5(4) . . . . ?
C3 C4 N4 C9 -157.0(3) . . . . ?
C3 C4 N4 C11 80.9(4) . . . . ?
C3 C4 N4 Pd1 -32.9(3) . . . . ?
C12 C11 N4 C9 -57.1(5) . . . . ?
C12 C11 N4 C4 65.0(5) . . . . ?
C12 C11 N4 Pd1 178.5(3) . . . . ?
F2 C13 S1 O5 -60.3(4) . . . . ?
F1 C13 S1 O5 60.9(4) . . . . ?
F3 C13 S1 O5 -179.0(3) . . . . ?
F2 C13 S1 O3 178.2(3) . . . . ?
F1 C13 S1 O3 -60.6(4) . . . . ?
F3 C13 S1 O3 59.6(3) . . . . ?
F2 C13 S1 O4 59.5(4) . . . . ?
F1 C13 S1 O4 -179.3(3) . . . . ?
F3 C13 S1 O4 -59.2(3) . . . . ?

_refine_diff_density_max         0.492
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.079

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_Pt_MS1h_200K
_database_code_depnum_ccdc_archive 'CCDC 1564467'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3256(2)
_cell_length_b                   12.9851(3)
_cell_length_c                   16.7595(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.118(2)
_cell_angle_gamma                90
_cell_volume                     2003.83(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9951
_cell_measurement_theta_min      3.9840
_cell_measurement_theta_max      29.6850

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 5 0.1067
-5 0 4 0.0512
1 5 -1 0.2318
-1 1 -5 0.1103
-1 -5 -3 0.2517
-1 0 -5 0.1033
5 0 -4 0.0348
0 -1 1 0.1437
-5 1 4 0.0508
-3 -5 2 0.1832
-3 5 2 0.1520
0 3 -5 0.1696
_exptl_absorpt_coefficient_mu    7.165
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            21897
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.371
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4091
_reflns_number_gt                3667
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0162P)²+1.1204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4091
_refine_ls_number_parameters     255
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0186
_refine_ls_wR_factor_ref         0.0415
_refine_ls_wR_factor_gt          0.0397
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_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 -0.0079(3) 0.5637(2) 0.81662(19) 0.0303(6) Uani 1 1 d . U . . .
H1A H -0.0971 0.5549 0.8388 0.036 Uiso 1 1 calc R U . . .
H1B H 0.0442 0.6220 0.8434 0.036 Uiso 1 1 calc R U . . .
C2 C -0.0432(3) 0.5845(2) 0.72743(19) 0.0306(6) Uani 1 1 d . U . . .
H2A H -0.1046 0.5305 0.7006 0.037 Uiso 1 1 calc R U . . .
H2B H -0.0934 0.6498 0.7176 0.037 Uiso 1 1 calc R U . . .
C3 C 0.0899(4) 0.5849(2) 0.60780(18) 0.0306(7) Uani 1 1 d . U . . .
H3A H 0.0552 0.6503 0.5843 0.037 Uiso 1 1 calc R U . . .
H3B H 0.0246 0.5309 0.5844 0.037 Uiso 1 1 calc R U . . .
C4 C 0.2420(4) 0.5642(2) 0.5925(2) 0.0315(7) Uani 1 1 d . U . . .
H4A H 0.3045 0.6214 0.6122 0.038 Uiso 1 1 calc R U . . .
H4B H 0.2422 0.5575 0.5349 0.038 Uiso 1 1 calc R U . . .
C5 C -0.0104(3) 0.3730(2) 0.81917(19) 0.0300(7) Uani 1 1 d . U . . .
H5A H 0.0525 0.3132 0.8221 0.036 Uiso 1 1 calc R U . . .
H5B H -0.0646 0.3757 0.7648 0.036 Uiso 1 1 calc R U . . .
C6 C -0.1176(4) 0.3568(3) 0.8774(2) 0.0435(9) Uani 1 1 d . U . . .
H6A H -0.1761 0.2972 0.8613 0.065 Uiso 1 1 calc R U . . .
H6B H -0.1791 0.4162 0.8767 0.065 Uiso 1 1 calc R U . . .
H6C H -0.0656 0.3466 0.9310 0.065 Uiso 1 1 calc R U . . .
C7 C 0.1648(4) 0.4685(2) 0.91709(19) 0.0307(7) Uani 1 1 d . U . . .
H7A H 0.2116 0.4022 0.9283 0.037 Uiso 1 1 calc R U . . .
H7B H 0.0954 0.4770 0.9540 0.037 Uiso 1 1 calc R U . . .
C8 C 0.2781(4) 0.5518(3) 0.9336(2) 0.0394(8) Uani 1 1 d . U . . .
H8A H 0.3419 0.5484 0.8940 0.059 Uiso 1 1 calc R U . . .
H8B H 0.3332 0.5423 0.9865 0.059 Uiso 1 1 calc R U . . .
H8C H 0.2314 0.6179 0.9307 0.059 Uiso 1 1 calc R U . . .
C9 C 0.2363(3) 0.3742(2) 0.58681(18) 0.0295(6) Uani 1 1 d . U . . .
H9A H 0.1312 0.3787 0.5798 0.035 Uiso 1 1 calc R U . . .
H9B H 0.2646 0.3130 0.6186 0.035 Uiso 1 1 calc R U . . .
C10 C 0.2805(4) 0.3596(3) 0.5038(2) 0.0387(8) Uani 1 1 d . U . . .
H10A H 0.2565 0.4204 0.4719 0.058 Uiso 1 1 calc R U . . .
H10B H 0.2297 0.3016 0.4774 0.058 Uiso 1 1 calc R U . . .
H10C H 0.3832 0.3476 0.5099 0.058 Uiso 1 1 calc R U . . .
C11 C 0.4608(3) 0.4634(2) 0.6435(2) 0.0343(7) Uani 1 1 d . U . . .
H11A H 0.4887 0.4701 0.5904 0.041 Uiso 1 1 calc R U . . .
H11B H 0.4942 0.3967 0.6649 0.041 Uiso 1 1 calc R U . . .
C12 C 0.5364(4) 0.5461(3) 0.6976(3) 0.0518(10) Uani 1 1 d . U . . .
H12A H 0.5259 0.6111 0.6700 0.078 Uiso 1 1 calc R U . . .
H12B H 0.6377 0.5296 0.7113 0.078 Uiso 1 1 calc R U . . .
H12C H 0.4939 0.5503 0.7461 0.078 Uiso 1 1 calc R U . . .
N2 N 0.0840(3) 0.46771(17) 0.83211(15) 0.0238(5) Uani 1 1 d . U . . .
N3 N 0.0980(3) 0.58737(18) 0.69718(14) 0.0239(5) Uani 1 1 d . U . . .
H3 H 0.1508 0.6494 0.7181 0.029 Uiso 1 1 calc R U . . .
N4 N 0.2985(3) 0.46669(17) 0.63474(15) 0.0238(5) Uani 1 1 d . U . . .
Pt1 Pt 0.21199(2) 0.46350(2) 0.74134(2) 0.01949(4) Uani 1 1 d . U . . .
N1 N 0.3124(2) 0.32816(16) 0.77951(13) 0.0303(5) Uani 0.106(4) 1 d D U P A 1
O1 O 0.2737(18) 0.2493(10) 0.7500(10) 0.0303(5) Uani 0.106(4) 1 d D U P A 1
O2 O 0.409(2) 0.3372(19) 0.8360(13) 0.0303(5) Uani 0.106(4) 1 d D U P A 1
N1A N 0.4395(4) 0.3230(3) 0.8275(2) 0.0413(10) Uani 0.894(4) 1 d D U P A 2
O1A O 0.3124(2) 0.32816(16) 0.77951(13) 0.0303(5) Uani 0.894(4) 1 d D U P A 2
O2A O 0.4899(3) 0.4058(2) 0.8495(2) 0.0569(9) Uani 0.894(4) 1 d D U P A 2
C13 C 0.6086(3) 0.6996(2) 0.90288(19) 0.0288(5) Uani 1 1 d . U . . .
F1 F 0.6530(2) 0.60228(13) 0.89950(12) 0.0417(5) Uani 1 1 d . U . . .
F2 F 0.5603(2) 0.71112(15) 0.97339(12) 0.0459(5) Uani 1 1 d . U . . .
F3 F 0.49485(19) 0.71216(14) 0.84441(12) 0.0404(5) Uani 1 1 d . U . . .
O3 O 0.8605(3) 0.76659(19) 0.96097(16) 0.0469(6) Uani 1 1 d . U . . .
O4 O 0.6820(3) 0.88853(16) 0.89602(14) 0.0381(5) Uani 1 1 d . U . . .
O5 O 0.7898(3) 0.76446(18) 0.81530(15) 0.0427(6) Uani 1 1 d . U . . .
S1 S 0.75251(8) 0.78970(6) 0.89256(5) 0.02901(17) Uani 1 1 d . 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
C1 C2 1.503(4) . ?
C1 N2 1.511(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.485(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.488(4) . ?
C3 C4 1.504(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.504(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.508(4) . ?
C5 C6 1.519(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.502(4) . ?
C7 C8 1.507(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.509(4) . ?
C9 C10 1.524(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.498(4) . ?
C11 C12 1.506(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N2 Pt1 2.078(2) . ?
N3 Pt1 2.004(2) . ?
N3 H3 0.9800 . ?
N4 Pt1 2.074(2) . ?
Pt1 O1A 2.046(2) . ?
Pt1 N1 2.046(2) . ?
N1 O1 1.170(9) . ?
N1 O2 1.207(9) . ?
N1A O2A 1.207(4) . ?
N1A O1A 1.325(4) . ?
C13 F1 1.334(3) . ?
C13 F3 1.335(3) . ?
C13 F2 1.338(4) . ?
C13 S1 1.809(3) . ?
O3 S1 1.433(2) . ?
O4 S1 1.447(2) . ?
O5 S1 1.431(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 N2 110.4(2) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.1(2) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.1(2) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 109.9(2) . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
N4 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 116.7(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 114.2(3) . . ?
N2 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 116.6(3) . . ?
N4 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N4 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 114.1(3) . . ?
N4 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
N4 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 N2 C5 109.6(2) . . ?
C7 N2 C1 110.1(2) . . ?
C5 N2 C1 110.2(2) . . ?
C7 N2 Pt1 115.76(19) . . ?
C5 N2 Pt1 105.27(17) . . ?
C1 N2 Pt1 105.77(17) . . ?
C2 N3 C3 115.9(2) . . ?
C2 N3 Pt1 107.53(17) . . ?
C3 N3 Pt1 107.09(17) . . ?
C2 N3 H3 108.7 . . ?
C3 N3 H3 108.7 . . ?
Pt1 N3 H3 108.7 . . ?
C11 N4 C4 110.1(2) . . ?
C11 N4 C9 109.1(2) . . ?
C4 N4 C9 110.1(2) . . ?
C11 N4 Pt1 116.1(2) . . ?
C4 N4 Pt1 105.48(17) . . ?
C9 N4 Pt1 105.87(17) . . ?
N3 Pt1 O1A 174.16(9) . . ?
N3 Pt1 N1 174.16(9) . . ?
N3 Pt1 N4 85.51(9) . . ?
O1A Pt1 N4 93.74(9) . . ?
N1 Pt1 N4 93.74(9) . . ?
N3 Pt1 N2 85.23(9) . . ?
O1A Pt1 N2 94.66(9) . . ?
N1 Pt1 N2 94.66(9) . . ?
N4 Pt1 N2 167.74(10) . . ?
O1 N1 O2 124.1(12) . . ?
O1 N1 Pt1 121.7(9) . . ?
O2 N1 Pt1 114.2(11) . . ?
O2A N1A O1A 114.0(3) . . ?
N1A O1A Pt1 123.7(2) . . ?
F1 C13 F3 107.5(2) . . ?
F1 C13 F2 107.1(2) . . ?
F3 C13 F2 107.1(2) . . ?
F1 C13 S1 111.6(2) . . ?
F3 C13 S1 111.5(2) . . ?
F2 C13 S1 111.8(2) . . ?
O5 S1 O3 115.82(16) . . ?
O5 S1 O4 114.60(14) . . ?
O3 S1 O4 114.83(15) . . ?
O5 S1 C13 103.21(14) . . ?
O3 S1 C13 103.07(15) . . ?
O4 S1 C13 102.76(14) . . ?

_refine_diff_density_max         0.676
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.091

####################################################################### 
# 
# 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_Pt_VT_130K
_database_code_depnum_ccdc_archive 'CCDC 1564468'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_Pt_VT_130K          
;
PROBLEM: Check Calcd Positive Residual Density on     Pt1       1.75 eA-3
RESPONSE: The residual density around the heavy Pt1 atom may be the result of fourier transform termination ripples, resulting from slightly reduced diffraction quality following a long period of photo-irradiation with this crystal (< 3 hrs).
;
# Added during the CSD deposition process: Tuesday 25 July 2017 11:25 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3072(4)
_cell_length_b                   13.0089(5)
_cell_length_c                   16.7706(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.852(5)
_cell_angle_gamma                90
_cell_volume                     2006.34(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    3168
_cell_measurement_theta_min      3.8060
_cell_measurement_theta_max      29.1790

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.156
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9270
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.365
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4094
_reflns_number_gt                3289
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0438P)²+1.3485P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4094
_refine_ls_number_parameters     257
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0914
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.017
_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 0.5125(7) 0.5628(5) 0.1852(4) 0.0334(13) Uani 1 1 d . U . . .
H1A H 0.6040 0.5535 0.1628 0.040 Uiso 1 1 calc R U . . .
H1B H 0.4601 0.6223 0.1578 0.040 Uiso 1 1 calc R U . . .
C2 C 0.5472(7) 0.5841(5) 0.2739(4) 0.0352(13) Uani 1 1 d . U . . .
H2A H 0.6113 0.5298 0.3013 0.042 Uiso 1 1 calc R U . . .
H2B H 0.5967 0.6513 0.2837 0.042 Uiso 1 1 calc R U . . .
C3 C 0.4103(8) 0.5858(6) 0.3931(4) 0.0372(14) Uani 1 1 d . U . . .
H3A H 0.4432 0.6536 0.4157 0.045 Uiso 1 1 calc R U . . .
H3B H 0.4780 0.5324 0.4186 0.045 Uiso 1 1 calc R U . . .
C4 C 0.2581(8) 0.5640(5) 0.4078(4) 0.0346(13) Uani 1 1 d . U . . .
H4A H 0.1936 0.6216 0.3870 0.042 Uiso 1 1 calc R U . . .
H4B H 0.2567 0.5578 0.4665 0.042 Uiso 1 1 calc R U . . .
C5 C 0.3398(8) 0.4676(5) 0.0847(4) 0.0353(14) Uani 1 1 d . U . . .
H5A H 0.2941 0.3995 0.0728 0.042 Uiso 1 1 calc R U . . .
H5B H 0.4109 0.4781 0.0472 0.042 Uiso 1 1 calc R U . . .
C6 C 0.2225(8) 0.5502(5) 0.0685(5) 0.0417(17) Uani 1 1 d . U . . .
H6A H 0.1732 0.5444 0.0127 0.063 Uiso 1 1 calc R U . . .
H6B H 0.2673 0.6182 0.0769 0.063 Uiso 1 1 calc R U . . .
H6C H 0.1516 0.5408 0.1055 0.063 Uiso 1 1 calc R U . . .
C7 C 0.5162(7) 0.3724(5) 0.1817(4) 0.0335(13) Uani 1 1 d . U . . .
H7A H 0.5724 0.3760 0.2368 0.040 Uiso 1 1 calc R U . . .
H7B H 0.4530 0.3110 0.1796 0.040 Uiso 1 1 calc R U . . .
C8 C 0.6223(8) 0.3567(6) 0.1228(5) 0.049(2) Uani 1 1 d . U . . .
H8A H 0.5685 0.3499 0.0681 0.074 Uiso 1 1 calc R U . . .
H8B H 0.6790 0.2941 0.1372 0.074 Uiso 1 1 calc R U . . .
H8C H 0.6880 0.4158 0.1252 0.074 Uiso 1 1 calc R U . . .
C9 C 0.0400(7) 0.4608(5) 0.3569(5) 0.0346(14) Uani 1 1 d . U . . .
H9A H 0.0079 0.3919 0.3365 0.042 Uiso 1 1 calc R U . . .
H9B H 0.0098 0.4694 0.4106 0.042 Uiso 1 1 calc R U . . .
C10 C -0.0351(9) 0.5409(6) 0.3006(6) 0.054(2) Uani 1 1 d . U . . .
H10A H 0.0083 0.5423 0.2510 0.082 Uiso 1 1 calc R U . . .
H10B H -0.0239 0.6084 0.3267 0.082 Uiso 1 1 calc R U . . .
H10C H -0.1387 0.5241 0.2875 0.082 Uiso 1 1 calc R U . . .
C11 C 0.2661(7) 0.3745(5) 0.4159(4) 0.0324(13) Uani 1 1 d . U . . .
H11A H 0.2397 0.3114 0.3841 0.039 Uiso 1 1 calc R U . . .
H11B H 0.3734 0.3802 0.4242 0.039 Uiso 1 1 calc R U . . .
C12 C 0.2188(8) 0.3615(6) 0.4971(4) 0.0411(16) Uani 1 1 d . U . . .
H12A H 0.1131 0.3523 0.4901 0.062 Uiso 1 1 calc R U . . .
H12B H 0.2460 0.4226 0.5301 0.062 Uiso 1 1 calc R U . . .
H12C H 0.2665 0.3009 0.5241 0.062 Uiso 1 1 calc R U . . .
N2 N 0.4192(6) 0.4668(4) 0.1688(3) 0.0305(9) Uani 1 1 d . U . . .
N3 N 0.4052(6) 0.5851(4) 0.3042(3) 0.0317(11) Uani 1 1 d . U . . .
H3 H 0.3508 0.6477 0.2820 0.038 Uiso 1 1 calc R U . . .
N4 N 0.2034(6) 0.4660(4) 0.3663(3) 0.0260(9) Uani 1 1 d . U . . .
Pt1 Pt 0.29175(2) 0.46219(2) 0.26010(2) 0.02527(10) Uani 1 1 d . U . . .
N1 N 0.1868(3) 0.3296(4) 0.22063(14) 0.0385(10) Uani 0.327(9) 1 d D U P A 1
O1 O 0.2360(7) 0.2500(8) 0.2426(3) 0.063(2) Uani 0.327(9) 1 d D U P A 1
O2 O 0.0744(8) 0.3404(12) 0.1747(4) 0.063(2) Uani 0.327(9) 1 d D U P A 1
N1A N 0.0645(7) 0.3197(6) 0.1712(3) 0.0385(10) Uani 0.635(9) 1 d D U P A 2
O1A O 0.1868(3) 0.3296(4) 0.22063(14) 0.0385(10) Uani 0.635(9) 1 d D U P A 2
O2A O 0.0130(7) 0.4075(5) 0.1481(4) 0.063(2) Uani 0.635(9) 1 d D U P A 2
O1B O 0.1868(3) 0.3296(4) 0.22063(14) 0.0385(10) Uani 0.038(9) 1 d D U P A 3
N1B N 0.0707(13) 0.359(3) 0.1727(5) 0.0385(10) Uani 0.038(9) 1 d D U P A 3
O2B O -0.0010(18) 0.278(4) 0.1456(8) 0.063(2) Uani 0.038(9) 1 d D U P A 3
C13 C 0.6082(7) 0.1979(5) 0.4033(4) 0.0316(9) Uani 1 1 d . U . . .
F1 F 0.6544(4) 0.1007(3) 0.4002(2) 0.0401(9) Uani 1 1 d . U . . .
F2 F 0.4944(4) 0.2099(3) 0.3451(2) 0.0393(9) Uani 1 1 d . U . . .
F3 F 0.5594(4) 0.2088(3) 0.4739(3) 0.0445(10) Uani 1 1 d . U . . .
O3 O 0.7902(5) 0.2634(3) 0.3156(3) 0.0403(11) Uani 1 1 d . U . . .
O4 O 0.6807(5) 0.3863(3) 0.3968(3) 0.0379(10) Uani 1 1 d . U . . .
O5 O 0.8605(5) 0.2651(4) 0.4618(3) 0.0443(11) Uani 1 1 d . U . . .
S1 S 0.75239(17) 0.28822(12) 0.39329(11) 0.0311(4) Uani 1 1 d . 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
C1 C2 1.498(10) . ?
C1 N2 1.521(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.488(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.483(8) . ?
C3 C4 1.501(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.502(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.488(9) . ?
C5 C6 1.525(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.514(9) . ?
C7 N2 1.520(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.504(10) . ?
C9 N4 1.506(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.504(9) . ?
C11 N4 1.517(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.077(5) . ?
N3 Pt1 1.994(5) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.074(5) . ?
Pt1 O1B 2.042(4) . ?
Pt1 O1A 2.042(4) . ?
Pt1 N1 2.042(4) . ?
N1 O1 1.169(8) . ?
N1 O2 1.208(8) . ?
N1A O2A 1.276(8) . ?
N1A O1A 1.307(7) . ?
O1B N1B 1.302(10) . ?
N1B O2B 1.299(10) . ?
C13 F2 1.334(7) . ?
C13 F1 1.339(7) . ?
C13 F3 1.340(8) . ?
C13 S1 1.811(6) . ?
O3 S1 1.437(5) . ?
O4 S1 1.446(5) . ?
O5 S1 1.437(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 111.2(5) . . ?
C2 C1 H1A 109.4 . . ?
N2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 105.9(5) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.2(6) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 110.2(5) . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
N4 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 114.3(5) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N2 116.7(6) . . ?
C8 C7 H7A 108.1 . . ?
N2 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
N2 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N4 113.5(5) . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
N4 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 116.4(5) . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11B 108.2 . . ?
N4 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C7 109.7(5) . . ?
C5 N2 C1 110.6(5) . . ?
C7 N2 C1 109.1(5) . . ?
C5 N2 Pt1 116.2(4) . . ?
C7 N2 Pt1 105.4(4) . . ?
C1 N2 Pt1 105.4(4) . . ?
C3 N3 C2 116.8(5) . . ?
C3 N3 Pt1 108.1(4) . . ?
C2 N3 Pt1 108.3(4) . . ?
C3 N3 H3 107.8 . . ?
C2 N3 H3 107.8 . . ?
Pt1 N3 H3 107.8 . . ?
C4 N4 C9 110.6(5) . . ?
C4 N4 C11 109.7(5) . . ?
C9 N4 C11 108.6(5) . . ?
C4 N4 Pt1 105.5(4) . . ?
C9 N4 Pt1 115.9(4) . . ?
C11 N4 Pt1 106.4(4) . . ?
N3 Pt1 O1B 175.59(19) . . ?
N3 Pt1 O1A 175.59(19) . . ?
N3 Pt1 N1 175.59(19) . . ?
N3 Pt1 N4 85.4(2) . . ?
O1B Pt1 N4 93.76(15) . . ?
O1A Pt1 N4 93.76(15) . . ?
N1 Pt1 N4 93.76(15) . . ?
N3 Pt1 N2 85.4(2) . . ?
O1B Pt1 N2 94.87(16) . . ?
O1A Pt1 N2 94.87(16) . . ?
N1 Pt1 N2 94.87(16) . . ?
N4 Pt1 N2 168.3(2) . . ?
O1 N1 O2 124.3(9) . . ?
O1 N1 Pt1 120.1(5) . . ?
O2 N1 Pt1 115.7(8) . . ?
O2A N1A O1A 110.7(7) . . ?
N1A O1A Pt1 128.0(5) . . ?
N1B O1B Pt1 105.1(18) . . ?
O2B N1B O1B 107.8(12) . . ?
F2 C13 F1 107.7(5) . . ?
F2 C13 F3 107.2(5) . . ?
F1 C13 F3 106.8(5) . . ?
F2 C13 S1 111.9(4) . . ?
F1 C13 S1 111.3(4) . . ?
F3 C13 S1 111.7(4) . . ?
O3 S1 O5 116.0(3) . . ?
O3 S1 O4 114.4(3) . . ?
O5 S1 O4 115.0(3) . . ?
O3 S1 C13 103.1(3) . . ?
O5 S1 C13 103.2(3) . . ?
O4 S1 C13 102.5(3) . . ?

_refine_diff_density_max         1.666
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.179

####################################################################### 
# 
# 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_Pt_VT_140K
_database_code_depnum_ccdc_archive 'CCDC 1564472'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_Pt_VT_140K          
;
PROBLEM: Check Calcd Positive Residual Density on     Pt1       1.64 eA-3
RESPONSE: The residual density around the heavy Pt1 atom may be the result of fourier transform termination ripples, resulting from slightly reduced diffraction quality following a long period of photo-irradiation with this crystal (< 3 hrs).
;
# Added during the CSD deposition process: Tuesday 25 July 2017 11:25 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3116(4)
_cell_length_b                   13.0129(5)
_cell_length_c                   16.7859(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.811(4)
_cell_angle_gamma                90
_cell_volume                     2009.96(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    3144
_cell_measurement_theta_min      3.8090
_cell_measurement_theta_max      29.2400

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.143
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9297
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.363
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4101
_reflns_number_gt                3274
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0410P)²+1.5414P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4101
_refine_ls_number_parameters     249
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0904
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.037
_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 0.5123(7) 0.5625(5) 0.1852(4) 0.0332(13) Uani 1 1 d . U . . .
H1A H 0.6038 0.5535 0.1627 0.040 Uiso 1 1 calc R U . . .
H1B H 0.4597 0.6219 0.1578 0.040 Uiso 1 1 calc R U . . .
C2 C 0.5474(7) 0.5839(5) 0.2742(4) 0.0358(14) Uani 1 1 d . U . . .
H2A H 0.6110 0.5295 0.3016 0.043 Uiso 1 1 calc R U . . .
H2B H 0.5972 0.6509 0.2840 0.043 Uiso 1 1 calc R U . . .
C3 C 0.4112(8) 0.5847(5) 0.3927(4) 0.0368(14) Uani 1 1 d . U . . .
H3A H 0.4456 0.6519 0.4159 0.044 Uiso 1 1 calc R U . . .
H3B H 0.4781 0.5305 0.4176 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2579(8) 0.5638(5) 0.4080(4) 0.0362(13) Uani 1 1 d . U . . .
H4A H 0.2566 0.5575 0.4667 0.043 Uiso 1 1 calc R U . . .
H4B H 0.1937 0.6216 0.3874 0.043 Uiso 1 1 calc R U . . .
C5 C 0.3405(7) 0.4685(5) 0.0843(4) 0.0334(13) Uani 1 1 d . U . . .
H5A H 0.2958 0.4004 0.0714 0.040 Uiso 1 1 calc R U . . .
H5B H 0.4118 0.4805 0.0472 0.040 Uiso 1 1 calc R U . . .
C6 C 0.2237(9) 0.5496(5) 0.0694(5) 0.0458(18) Uani 1 1 d . U . . .
H6A H 0.1690 0.5410 0.0151 0.069 Uiso 1 1 calc R U . . .
H6B H 0.2685 0.6179 0.0741 0.069 Uiso 1 1 calc R U . . .
H6C H 0.1576 0.5426 0.1092 0.069 Uiso 1 1 calc R U . . .
C7 C 0.5152(7) 0.3723(5) 0.1816(4) 0.0354(14) Uani 1 1 d . U . . .
H7A H 0.4516 0.3111 0.1792 0.043 Uiso 1 1 calc R U . . .
H7B H 0.5711 0.3756 0.2366 0.043 Uiso 1 1 calc R U . . .
C8 C 0.6214(8) 0.3563(6) 0.1230(5) 0.050(2) Uani 1 1 d . U . . .
H8A H 0.5684 0.3541 0.0679 0.075 Uiso 1 1 calc R U . . .
H8B H 0.6733 0.2914 0.1353 0.075 Uiso 1 1 calc R U . . .
H8C H 0.6912 0.4132 0.1279 0.075 Uiso 1 1 calc R U . . .
C9 C 0.0405(7) 0.4614(5) 0.3568(5) 0.0379(15) Uani 1 1 d . U . . .
H9A H 0.0103 0.4708 0.4104 0.045 Uiso 1 1 calc R U . . .
H9B H 0.0078 0.3924 0.3369 0.045 Uiso 1 1 calc R U . . .
C10 C -0.0345(9) 0.5409(6) 0.3000(6) 0.059(2) Uani 1 1 d . U . . .
H10A H 0.0067 0.5401 0.2497 0.089 Uiso 1 1 calc R U . . .
H10B H -0.0204 0.6091 0.3249 0.089 Uiso 1 1 calc R U . . .
H10C H -0.1386 0.5255 0.2885 0.089 Uiso 1 1 calc R U . . .
C11 C 0.2656(7) 0.3754(5) 0.4159(4) 0.0349(13) Uani 1 1 d . U . . .
H11A H 0.3728 0.3814 0.4238 0.042 Uiso 1 1 calc R U . . .
H11B H 0.2396 0.3121 0.3841 0.042 Uiso 1 1 calc R U . . .
C12 C 0.2194(7) 0.3613(6) 0.4978(4) 0.0422(17) Uani 1 1 d . U . . .
H12A H 0.1141 0.3506 0.4912 0.063 Uiso 1 1 calc R U . . .
H12B H 0.2451 0.4228 0.5306 0.063 Uiso 1 1 calc R U . . .
H12C H 0.2692 0.3015 0.5246 0.063 Uiso 1 1 calc R U . . .
N2 N 0.4195(6) 0.4664(4) 0.1690(3) 0.0303(9) Uani 1 1 d . U . . .
N3 N 0.4058(6) 0.5852(4) 0.3041(3) 0.0323(11) Uani 1 1 d . U . . .
H3 H 0.3516 0.6480 0.2822 0.039 Uiso 1 1 calc R U . . .
N4 N 0.2031(6) 0.4657(4) 0.3662(3) 0.0278(9) Uani 1 1 d . U . . .
Pt1 Pt 0.29193(2) 0.46214(2) 0.26020(2) 0.02617(10) Uani 1 1 d . U . . .
N1 N 0.1872(3) 0.3293(4) 0.22088(16) 0.0396(10) Uani 0.343(8) 1 d D U P A 1
O1 O 0.2346(8) 0.2495(8) 0.2419(4) 0.070(2) Uani 0.343(8) 1 d D U P A 1
O2 O 0.0755(8) 0.3432(11) 0.1753(4) 0.070(2) Uani 0.343(8) 1 d D U P A 1
N1A N 0.0648(7) 0.3192(6) 0.1715(3) 0.0396(10) Uani 0.657(8) 1 d D U P A 2
O1A O 0.1872(3) 0.3293(4) 0.22088(16) 0.0396(10) Uani 0.657(8) 1 d D U P A 2
O2A O 0.0133(7) 0.4067(5) 0.1486(4) 0.070(2) Uani 0.657(8) 1 d D U P A 2
C13 C 0.6086(7) 0.1979(5) 0.4041(4) 0.0318(9) Uani 1 1 d . U . . .
F1 F 0.6538(4) 0.1009(3) 0.4007(3) 0.0414(9) Uani 1 1 d . U . . .
F2 F 0.4950(4) 0.2098(3) 0.3456(3) 0.0412(9) Uani 1 1 d . U . . .
F3 F 0.5587(4) 0.2086(3) 0.4739(3) 0.0472(10) Uani 1 1 d . U . . .
O3 O 0.7900(5) 0.2633(4) 0.3160(3) 0.0421(11) Uani 1 1 d . U . . .
O4 O 0.6809(5) 0.3866(3) 0.3970(3) 0.0404(11) Uani 1 1 d . U . . .
O5 O 0.8596(5) 0.2644(4) 0.4618(3) 0.0475(12) Uani 1 1 d . U . . .
S1 S 0.75234(17) 0.28818(12) 0.39337(11) 0.0326(4) Uani 1 1 d . 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
C1 C2 1.507(10) . ?
C1 N2 1.521(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.481(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.481(8) . ?
C3 C4 1.513(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.507(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.497(9) . ?
C5 C6 1.509(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.509(8) . ?
C7 C8 1.511(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.500(8) . ?
C9 C10 1.504(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.505(8) . ?
C11 C12 1.513(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.078(5) . ?
N3 Pt1 1.998(5) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.074(5) . ?
Pt1 O1A 2.044(4) . ?
Pt1 N1 2.044(4) . ?
N1 O1 1.162(8) . ?
N1 O2 1.207(8) . ?
N1A O2A 1.272(8) . ?
N1A O1A 1.309(7) . ?
C13 F3 1.333(8) . ?
C13 F1 1.334(7) . ?
C13 F2 1.338(7) . ?
C13 S1 1.811(6) . ?
O3 S1 1.433(5) . ?
O4 S1 1.449(5) . ?
O5 S1 1.436(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 111.1(5) . . ?
C2 C1 H1A 109.4 . . ?
N2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 105.6(5) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.8 . . ?
N3 C3 C4 106.4(6) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 109.5(5) . . ?
N4 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N4 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.1(6) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.9(6) . . ?
N2 C7 H7A 108.1 . . ?
C8 C7 H7A 108.1 . . ?
N2 C7 H7B 108.1 . . ?
C8 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.9(6) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 117.2(5) . . ?
N4 C11 H11A 108.0 . . ?
C12 C11 H11A 108.0 . . ?
N4 C11 H11B 108.0 . . ?
C12 C11 H11B 108.0 . . ?
H11A C11 H11B 107.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C7 110.0(5) . . ?
C5 N2 C1 109.7(5) . . ?
C7 N2 C1 109.6(5) . . ?
C5 N2 Pt1 116.5(4) . . ?
C7 N2 Pt1 105.5(4) . . ?
C1 N2 Pt1 105.3(4) . . ?
C2 N3 C3 116.4(5) . . ?
C2 N3 Pt1 108.4(4) . . ?
C3 N3 Pt1 107.5(4) . . ?
C2 N3 H3 108.1 . . ?
C3 N3 H3 108.1 . . ?
Pt1 N3 H3 108.1 . . ?
C9 N4 C11 109.2(5) . . ?
C9 N4 C4 110.1(5) . . ?
C11 N4 C4 109.2(5) . . ?
C9 N4 Pt1 116.0(4) . . ?
C11 N4 Pt1 106.6(4) . . ?
C4 N4 Pt1 105.5(4) . . ?
N3 Pt1 O1A 175.5(2) . . ?
N3 Pt1 N1 175.5(2) . . ?
N3 Pt1 N4 85.7(2) . . ?
O1A Pt1 N4 93.59(16) . . ?
N1 Pt1 N4 93.59(16) . . ?
N3 Pt1 N2 85.4(2) . . ?
O1A Pt1 N2 94.77(16) . . ?
N1 Pt1 N2 94.77(16) . . ?
N4 Pt1 N2 168.4(2) . . ?
O1 N1 O2 125.2(9) . . ?
O1 N1 Pt1 121.2(5) . . ?
O2 N1 Pt1 113.6(8) . . ?
O2A N1A O1A 110.6(7) . . ?
N1A O1A Pt1 128.0(5) . . ?
F3 C13 F1 106.9(5) . . ?
F3 C13 F2 106.9(5) . . ?
F1 C13 F2 107.3(5) . . ?
F3 C13 S1 112.4(4) . . ?
F1 C13 S1 111.6(4) . . ?
F2 C13 S1 111.4(5) . . ?
O3 S1 O5 116.1(3) . . ?
O3 S1 O4 114.5(3) . . ?
O5 S1 O4 115.1(3) . . ?
O3 S1 C13 103.3(3) . . ?
O5 S1 C13 102.4(3) . . ?
O4 S1 C13 102.6(3) . . ?

_refine_diff_density_max         1.745
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.175

####################################################################### 
# 
# 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_Pt_MS1h_100K
_database_code_depnum_ccdc_archive 'CCDC 1564474'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2898(5)
_cell_length_b                   13.0891(5)
_cell_length_c                   16.8662(11)
_cell_angle_alpha                90
_cell_angle_beta                 98.239(5)
_cell_angle_gamma                90
_cell_volume                     2029.68(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2975
_cell_measurement_theta_min      4.3290
_cell_measurement_theta_max      29.2150

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.074
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.234
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9917
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.344
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4145
_reflns_number_gt                3433
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0284P)²+5.9567P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4145
_refine_ls_number_parameters     257
_refine_ls_number_restraints     292
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0708
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.022
_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 0.5236(7) 0.5597(4) 0.1887(4) 0.0296(12) Uani 1 1 d . U . . .
H1A H 0.4712 0.6189 0.1618 0.035 Uiso 1 1 calc R U . . .
H1B H 0.6156 0.5508 0.1663 0.035 Uiso 1 1 calc R U . . .
C2 C 0.5571(7) 0.5803(5) 0.2787(4) 0.0303(12) Uani 1 1 d . U . . .
H2A H 0.6195 0.5256 0.3058 0.036 Uiso 1 1 calc R U . . .
H2B H 0.6075 0.6466 0.2890 0.036 Uiso 1 1 calc R U . . .
C3 C 0.4146(7) 0.5843(5) 0.3958(4) 0.0304(12) Uani 1 1 d . U . . .
H3A H 0.4474 0.6518 0.4179 0.036 Uiso 1 1 calc R U . . .
H3B H 0.4802 0.5311 0.4223 0.036 Uiso 1 1 calc R U . . .
C4 C 0.2581(7) 0.5640(4) 0.4082(4) 0.0290(12) Uani 1 1 d . U . . .
H4A H 0.2518 0.5606 0.4663 0.035 Uiso 1 1 calc R U . . .
H4B H 0.1950 0.6206 0.3849 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3516(7) 0.4664(4) 0.0895(4) 0.0305(12) Uani 1 1 d . U . . .
H5A H 0.3102 0.3978 0.0761 0.037 Uiso 1 1 calc R U . . .
H5B H 0.4222 0.4811 0.0523 0.037 Uiso 1 1 calc R U . . .
C6 C 0.2302(8) 0.5443(5) 0.0761(4) 0.0397(15) Uani 1 1 d . U . . .
H6A H 0.1790 0.5379 0.0213 0.060 Uiso 1 1 calc R U . . .
H6B H 0.2711 0.6132 0.0839 0.060 Uiso 1 1 calc R U . . .
H6C H 0.1618 0.5324 0.1143 0.060 Uiso 1 1 calc R U . . .
C7 C 0.5269(7) 0.3704(4) 0.1849(4) 0.0316(12) Uani 1 1 d . U . . .
H7A H 0.4635 0.3093 0.1823 0.038 Uiso 1 1 calc R U . . .
H7B H 0.5825 0.3731 0.2395 0.038 Uiso 1 1 calc R U . . .
C8 C 0.6337(8) 0.3561(5) 0.1258(4) 0.0456(18) Uani 1 1 d . U . . .
H8A H 0.5802 0.3471 0.0718 0.068 Uiso 1 1 calc R U . . .
H8B H 0.6935 0.2955 0.1406 0.068 Uiso 1 1 calc R U . . .
H8C H 0.6964 0.4164 0.1268 0.068 Uiso 1 1 calc R U . . .
C9 C 0.0453(7) 0.4588(5) 0.3582(4) 0.0323(12) Uani 1 1 d . U . . .
H9A H 0.0123 0.4728 0.4104 0.039 Uiso 1 1 calc R U . . .
H9B H 0.0149 0.3884 0.3421 0.039 Uiso 1 1 calc R U . . .
C10 C -0.0304(8) 0.5334(6) 0.2960(5) 0.052(2) Uani 1 1 d . U . . .
H10A H 0.0021 0.5206 0.2441 0.079 Uiso 1 1 calc R U . . .
H10B H -0.0058 0.6036 0.3130 0.079 Uiso 1 1 calc R U . . .
H10C H -0.1359 0.5238 0.2909 0.079 Uiso 1 1 calc R U . . .
C11 C 0.2681(7) 0.3747(4) 0.4193(4) 0.0302(12) Uani 1 1 d . U . . .
H11A H 0.2424 0.3111 0.3888 0.036 Uiso 1 1 calc R U . . .
H11B H 0.3755 0.3803 0.4277 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2176(7) 0.3650(5) 0.5001(4) 0.0384(15) Uani 1 1 d . U . . .
H12A H 0.1119 0.3553 0.4928 0.058 Uiso 1 1 calc R U . . .
H12B H 0.2428 0.4272 0.5313 0.058 Uiso 1 1 calc R U . . .
H12C H 0.2651 0.3061 0.5286 0.058 Uiso 1 1 calc R U . . .
N2 N 0.4308(6) 0.4642(3) 0.1731(3) 0.0253(8) Uani 1 1 d . U . . .
N3 N 0.4139(5) 0.5820(3) 0.3076(3) 0.0253(9) Uani 1 1 d . U . . .
H3 H 0.3606 0.6440 0.2846 0.030 Uiso 1 1 calc R U . . .
N4 N 0.2065(5) 0.4643(3) 0.3687(3) 0.0231(8) Uani 1 1 d . U . . .
Pt1 Pt 0.30035(2) 0.45925(2) 0.26379(2) 0.02135(8) Uani 1 1 d . U . . .
N1 N 0.1913(3) 0.3311(3) 0.22303(14) 0.0300(9) Uani 0.710(8) 1 d D U P A 1
O1 O 0.2327(6) 0.2518(5) 0.2520(3) 0.071(2) Uani 0.710(8) 1 d D U P A 1
O2 O 0.0870(6) 0.3361(6) 0.1705(3) 0.071(2) Uani 0.710(8) 1 d D U P A 1
N1A N 0.0785(8) 0.3172(11) 0.1683(4) 0.0300(9) Uani 0.224(9) 1 d D U P A 2
O1A O 0.1913(3) 0.3311(3) 0.22303(14) 0.0300(9) Uani 0.224(9) 1 d D U P A 2
O2A O 0.0387(12) 0.4061(12) 0.1391(6) 0.071(2) Uani 0.224(9) 1 d D U P A 2
O1B O 0.1913(3) 0.3311(3) 0.22303(14) 0.0300(9) Uani 0.066(8) 1 d D U P A 3
N1B N 0.0944(14) 0.375(2) 0.1702(6) 0.0300(9) Uani 0.066(8) 1 d D U P A 3
O2B O 0.0105(10) 0.303(3) 0.1360(7) 0.071(2) Uani 0.066(8) 1 d D U P A 3
C13 C 0.6090(6) 0.1938(4) 0.4061(4) 0.0266(8) Uani 1 1 d . U . . .
F1 F 0.6569(4) 0.0976(2) 0.4033(2) 0.0341(8) Uani 1 1 d . U . . .
F2 F 0.4975(4) 0.2052(3) 0.3478(2) 0.0362(8) Uani 1 1 d . U . . .
F3 F 0.5583(4) 0.2047(3) 0.4760(2) 0.0384(8) Uani 1 1 d . U . . .
O3 O 0.7937(5) 0.2605(3) 0.3191(3) 0.0360(10) Uani 1 1 d . U . . .
O4 O 0.6803(5) 0.3821(3) 0.3996(2) 0.0313(9) Uani 1 1 d . U . . .
O5 O 0.8603(5) 0.2624(3) 0.4642(3) 0.0397(10) Uani 1 1 d . U . . .
S1 S 0.75359(16) 0.28467(10) 0.39602(9) 0.0264(3) Uani 1 1 d . 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
C1 N2 1.520(7) . ?
C1 C2 1.529(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.482(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.486(7) . ?
C3 C4 1.522(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.513(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.494(8) . ?
C5 C6 1.514(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.514(7) . ?
C7 C8 1.515(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.484(8) . ?
C9 C10 1.529(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.509(8) . ?
C11 N4 1.514(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.084(5) . ?
N3 Pt1 2.004(4) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.082(5) . ?
Pt1 O1B 2.028(4) . ?
Pt1 O1A 2.028(4) . ?
Pt1 N1 2.028(4) . ?
Pt1 N1B 2.55(2) . ?
N1 O1 1.188(6) . ?
N1 O2 1.217(6) . ?
N1A O2A 1.297(10) . ?
N1A O1A 1.306(9) . ?
O1B N1B 1.304(10) . ?
N1B O2B 1.303(10) . ?
C13 F2 1.331(7) . ?
C13 F1 1.339(6) . ?
C13 F3 1.339(7) . ?
C13 S1 1.820(6) . ?
O3 S1 1.435(4) . ?
O4 S1 1.451(4) . ?
O5 S1 1.437(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 110.3(5) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.3(5) . . ?
N3 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
N3 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
N3 C3 C4 105.5(5) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.8 . . ?
N4 C4 C3 109.8(5) . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.2(5) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.3(5) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 114.1(5) . . ?
N4 C9 H9A 108.7 . . ?
C10 C9 H9A 108.7 . . ?
N4 C9 H9B 108.7 . . ?
C10 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 115.7(5) . . ?
C12 C11 H11A 108.4 . . ?
N4 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
N4 C11 H11B 108.4 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C7 109.9(4) . . ?
C5 N2 C1 109.7(4) . . ?
C7 N2 C1 109.6(5) . . ?
C5 N2 Pt1 115.7(4) . . ?
C7 N2 Pt1 105.8(3) . . ?
C1 N2 Pt1 105.8(3) . . ?
C2 N3 C3 117.0(5) . . ?
C2 N3 Pt1 108.4(3) . . ?
C3 N3 Pt1 108.2(3) . . ?
C2 N3 H3 107.6 . . ?
C3 N3 H3 107.6 . . ?
Pt1 N3 H3 107.6 . . ?
C9 N4 C4 110.2(4) . . ?
C9 N4 C11 108.8(4) . . ?
C4 N4 C11 110.5(5) . . ?
C9 N4 Pt1 115.8(4) . . ?
C4 N4 Pt1 104.9(3) . . ?
C11 N4 Pt1 106.5(3) . . ?
N3 Pt1 O1B 177.43(17) . . ?
N3 Pt1 O1A 177.43(17) . . ?
N3 Pt1 N1 177.43(17) . . ?
N3 Pt1 N4 85.61(18) . . ?
O1B Pt1 N4 93.70(14) . . ?
O1A Pt1 N4 93.70(14) . . ?
N1 Pt1 N4 93.70(14) . . ?
N3 Pt1 N2 85.14(18) . . ?
O1B Pt1 N2 95.25(14) . . ?
O1A Pt1 N2 95.25(14) . . ?
N1 Pt1 N2 95.25(14) . . ?
N4 Pt1 N2 168.75(19) . . ?
N3 Pt1 N1B 152.1(5) . . ?
O1B Pt1 N1B 30.4(5) . . ?
N4 Pt1 N1B 99.87(19) . . ?
N2 Pt1 N1B 91.29(19) . . ?
O1 N1 O2 121.6(5) . . ?
O1 N1 Pt1 117.8(3) . . ?
O2 N1 Pt1 120.6(5) . . ?
O2A N1A O1A 107.4(10) . . ?
N1A O1A Pt1 131.8(7) . . ?
N1B O1B Pt1 97.6(13) . . ?
O2B N1B O1B 107.3(11) . . ?
O2B N1B Pt1 159.3(12) . . ?
O1B N1B Pt1 51.9(9) . . ?
F2 C13 F1 107.9(5) . . ?
F2 C13 F3 107.7(5) . . ?
F1 C13 F3 107.0(4) . . ?
F2 C13 S1 111.4(4) . . ?
F1 C13 S1 111.0(4) . . ?
F3 C13 S1 111.7(4) . . ?
O3 S1 O5 116.1(3) . . ?
O3 S1 O4 114.5(2) . . ?
O5 S1 O4 114.8(3) . . ?
O3 S1 C13 103.4(3) . . ?
O5 S1 C13 103.1(3) . . ?
O4 S1 C13 102.3(3) . . ?

_refine_diff_density_max         2.190
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.159

####################################################################### 
# 
# 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_Pt_GS_100K
_database_code_depnum_ccdc_archive 'CCDC 1564462'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2331(3)
_cell_length_b                   13.1391(4)
_cell_length_c                   16.9695(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.100(3)
_cell_angle_gamma                90
_cell_volume                     2042.86(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4869
_cell_measurement_theta_min      3.9280
_cell_measurement_theta_max      29.4290

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.028
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            10322
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.329
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4173
_reflns_number_gt                3598
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0320P)²+3.3151P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4173
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0627
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 0.5355(6) 0.5557(3) 0.1937(3) 0.0264(11) Uani 1 1 d . . . . .
H1A H 0.6296 0.5466 0.1722 0.032 Uiso 1 1 calc R U . . .
H1B H 0.4841 0.6142 0.1661 0.032 Uiso 1 1 calc R U . . .
C2 C 0.5638(5) 0.5776(4) 0.2814(3) 0.0247(11) Uani 1 1 d . . . . .
H2A H 0.6259 0.5239 0.3091 0.030 Uiso 1 1 calc R U . . .
H2B H 0.6134 0.6440 0.2911 0.030 Uiso 1 1 calc R U . . .
C3 C 0.4134(6) 0.5844(4) 0.3962(3) 0.0236(10) Uani 1 1 d . . . . .
H3A H 0.4432 0.6527 0.4169 0.028 Uiso 1 1 calc R U . . .
H3B H 0.4792 0.5330 0.4242 0.028 Uiso 1 1 calc R U . . .
C4 C 0.2577(6) 0.5631(3) 0.4077(3) 0.0240(10) Uani 1 1 d . . . . .
H4A H 0.1943 0.6182 0.3832 0.029 Uiso 1 1 calc R U . . .
H4B H 0.2482 0.5613 0.4652 0.029 Uiso 1 1 calc R U . . .
C5 C 0.3665(6) 0.4638(4) 0.0944(3) 0.0284(11) Uani 1 1 d . . . . .
H5A H 0.3282 0.3951 0.0798 0.034 Uiso 1 1 calc R U . . .
H5B H 0.4379 0.4817 0.0577 0.034 Uiso 1 1 calc R U . . .
C6 C 0.2418(7) 0.5391(4) 0.0834(3) 0.0350(13) Uani 1 1 d . . . . .
H6A H 0.1978 0.5386 0.0278 0.052 Uiso 1 1 calc R U . . .
H6B H 0.2787 0.6075 0.0977 0.052 Uiso 1 1 calc R U . . .
H6C H 0.1682 0.5201 0.1177 0.052 Uiso 1 1 calc R U . . .
C7 C 0.5400(6) 0.3680(4) 0.1891(3) 0.0288(11) Uani 1 1 d . . . . .
H7A H 0.4766 0.3070 0.1869 0.035 Uiso 1 1 calc R U . . .
H7B H 0.5953 0.3708 0.2428 0.035 Uiso 1 1 calc R U . . .
C8 C 0.6476(7) 0.3543(4) 0.1295(4) 0.0468(16) Uani 1 1 d . . . . .
H8A H 0.5944 0.3436 0.0765 0.070 Uiso 1 1 calc R U . . .
H8B H 0.7096 0.2952 0.1444 0.070 Uiso 1 1 calc R U . . .
H8C H 0.7085 0.4153 0.1291 0.070 Uiso 1 1 calc R U . . .
C9 C 0.0474(5) 0.4554(4) 0.3585(3) 0.0298(12) Uani 1 1 d . . . . .
H9A H 0.0103 0.4726 0.4092 0.036 Uiso 1 1 calc R U . . .
H9B H 0.0197 0.3840 0.3456 0.036 Uiso 1 1 calc R U . . .
C10 C -0.0272(6) 0.5239(5) 0.2936(4) 0.0450(15) Uani 1 1 d . . . . .
H10A H 0.0087 0.5077 0.2431 0.068 Uiso 1 1 calc R U . . .
H10B H -0.0053 0.5952 0.3073 0.068 Uiso 1 1 calc R U . . .
H10C H -0.1329 0.5131 0.2887 0.068 Uiso 1 1 calc R U . . .
C11 C 0.2721(5) 0.3764(3) 0.4236(3) 0.0242(10) Uani 1 1 d . . . . .
H11A H 0.3795 0.3842 0.4327 0.029 Uiso 1 1 calc R U . . .
H11B H 0.2508 0.3113 0.3950 0.029 Uiso 1 1 calc R U . . .
C12 C 0.2157(6) 0.3689(4) 0.5039(3) 0.0327(12) Uani 1 1 d . . . . .
H12A H 0.1106 0.3551 0.4961 0.049 Uiso 1 1 calc R U . . .
H12B H 0.2339 0.4333 0.5326 0.049 Uiso 1 1 calc R U . . .
H12C H 0.2663 0.3136 0.5348 0.049 Uiso 1 1 calc R U . . .
N1 N 0.2013(4) 0.3300(3) 0.2261(2) 0.0243(9) Uani 1 1 d . . . . .
N2 N 0.4439(5) 0.4607(3) 0.1780(2) 0.0219(9) Uani 1 1 d . . . . .
N3 N 0.4191(4) 0.5793(3) 0.3097(2) 0.0175(8) Uani 1 1 d . . . . .
H3 H 0.3658 0.6401 0.2854 0.021 Uiso 1 1 calc R U . . .
N4 N 0.2096(4) 0.4626(3) 0.3704(2) 0.0193(8) Uani 1 1 d . . . . .
O1 O 0.2286(6) 0.2494(3) 0.2593(3) 0.0663(11) Uani 1 1 d . . . . .
O2 O 0.1035(6) 0.3309(3) 0.1702(3) 0.0663(11) Uani 1 1 d . . . . .
Pt1 Pt 0.30871(2) 0.45553(2) 0.26723(2) 0.01613(7) Uani 1 1 d . . . . .
C13 C 0.6097(5) 0.1901(4) 0.4101(3) 0.0246(11) Uani 1 1 d . . . . .
F1 F 0.6582(3) 0.09464(19) 0.40774(18) 0.0328(7) Uani 1 1 d . . . . .
F2 F 0.4997(3) 0.2001(2) 0.35199(18) 0.0362(7) Uani 1 1 d . . . . .
F3 F 0.5550(3) 0.2013(2) 0.47870(17) 0.0363(7) Uani 1 1 d . . . . .
O3 O 0.7953(4) 0.2574(3) 0.3226(2) 0.0328(8) Uani 1 1 d . . . . .
O4 O 0.6789(4) 0.3784(2) 0.40278(19) 0.0276(8) Uani 1 1 d . . . . .
O5 O 0.8594(4) 0.2605(3) 0.4668(2) 0.0385(10) Uani 1 1 d . . . . .
S1 S 0.75303(13) 0.28187(9) 0.39947(7) 0.0231(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.508(7) . ?
C1 N2 1.512(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.475(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.477(6) . ?
C3 C4 1.501(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.507(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.508(6) . ?
C5 C6 1.511(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.504(6) . ?
C7 C8 1.513(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.489(6) . ?
C9 C10 1.520(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.519(6) . ?
C11 C12 1.521(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 O1 1.211(6) . ?
N1 O2 1.227(5) . ?
N1 Pt1 2.005(4) . ?
N2 Pt1 2.079(4) . ?
N3 Pt1 2.005(4) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.075(4) . ?
C13 F2 1.332(5) . ?
C13 F3 1.333(5) . ?
C13 F1 1.334(5) . ?
C13 S1 1.815(5) . ?
O3 S1 1.443(4) . ?
O4 S1 1.445(3) . ?
O5 S1 1.439(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 110.9(4) . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 105.7(4) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.8(4) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 110.3(4) . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
N4 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 113.6(4) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.0(4) . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 114.7(4) . . ?
N4 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N4 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 115.7(4) . . ?
N4 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N4 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 N1 O2 117.4(4) . . ?
O1 N1 Pt1 119.5(3) . . ?
O2 N1 Pt1 123.1(3) . . ?
C7 N2 C5 110.1(4) . . ?
C7 N2 C1 109.8(4) . . ?
C5 N2 C1 109.4(4) . . ?
C7 N2 Pt1 106.3(3) . . ?
C5 N2 Pt1 115.3(3) . . ?
C1 N2 Pt1 105.8(3) . . ?
C2 N3 C3 117.9(4) . . ?
C2 N3 Pt1 108.1(3) . . ?
C3 N3 Pt1 108.4(3) . . ?
C2 N3 H3 107.3 . . ?
C3 N3 H3 107.3 . . ?
Pt1 N3 H3 107.3 . . ?
C9 N4 C4 110.6(4) . . ?
C9 N4 C11 109.5(3) . . ?
C4 N4 C11 109.4(4) . . ?
C9 N4 Pt1 115.1(3) . . ?
C4 N4 Pt1 104.8(3) . . ?
C11 N4 Pt1 107.1(3) . . ?
N1 Pt1 N3 178.84(15) . . ?
N1 Pt1 N4 94.57(15) . . ?
N3 Pt1 N4 85.29(15) . . ?
N1 Pt1 N2 95.11(15) . . ?
N3 Pt1 N2 84.90(15) . . ?
N4 Pt1 N2 168.50(15) . . ?
F2 C13 F3 107.4(4) . . ?
F2 C13 F1 107.4(4) . . ?
F3 C13 F1 107.1(4) . . ?
F2 C13 S1 111.1(3) . . ?
F3 C13 S1 111.9(3) . . ?
F1 C13 S1 111.7(3) . . ?
O5 S1 O3 116.1(2) . . ?
O5 S1 O4 114.9(2) . . ?
O3 S1 O4 114.4(2) . . ?
O5 S1 C13 103.1(2) . . ?
O3 S1 C13 102.9(2) . . ?
O4 S1 C13 103.0(2) . . ?

_refine_diff_density_max         2.551
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.144

####################################################################### 
# 
# 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_Pt_VT_120K
_database_code_depnum_ccdc_archive 'CCDC 1564469'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_Pt_VT_120K          
;
PROBLEM: Check Calcd Residual Density  0.95A From     Pt1       2.10 eA-3
RESPONSE: The residual density around the heavy Pt1 atom may be the result of fourier transform termination ripples, resulting from slightly reduced diffraction quality following a long period of photo-irradiation with this crystal (< 3 hrs).
;
# Added during the CSD deposition process: Tuesday 25 July 2017 11:25 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3067(4)
_cell_length_b                   13.0094(5)
_cell_length_c                   16.7577(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.924(4)
_cell_angle_gamma                90
_cell_volume                     2004.37(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3205
_cell_measurement_theta_min      3.8820
_cell_measurement_theta_max      29.2910

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.163
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9222
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.365
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4091
_reflns_number_gt                3292
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0462P)²+0.7792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4091
_refine_ls_number_parameters     257
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.025
_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 0.5111(8) 0.5627(5) 0.1848(4) 0.0327(13) Uani 1 1 d . U . . .
H1A H 0.4578 0.6223 0.1579 0.039 Uiso 1 1 calc R U . . .
H1B H 0.6021 0.5541 0.1618 0.039 Uiso 1 1 calc R U . . .
C2 C 0.5482(7) 0.5841(5) 0.2748(4) 0.0327(14) Uani 1 1 d . U . . .
H2A H 0.6121 0.5296 0.3020 0.039 Uiso 1 1 calc R U . . .
H2B H 0.5981 0.6512 0.2846 0.039 Uiso 1 1 calc R U . . .
C3 C 0.4101(8) 0.5849(6) 0.3933(4) 0.0370(15) Uani 1 1 d . U . . .
H3A H 0.4440 0.6522 0.4165 0.044 Uiso 1 1 calc R U . . .
H3B H 0.4769 0.5308 0.4186 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2575(8) 0.5640(5) 0.4079(5) 0.0363(14) Uani 1 1 d . U . . .
H4A H 0.1934 0.6218 0.3870 0.044 Uiso 1 1 calc R U . . .
H4B H 0.2559 0.5577 0.4666 0.044 Uiso 1 1 calc R U . . .
C5 C 0.3408(8) 0.4682(5) 0.0847(4) 0.0339(14) Uani 1 1 d . U . . .
H5A H 0.2960 0.3998 0.0726 0.041 Uiso 1 1 calc R U . . .
H5B H 0.4119 0.4793 0.0473 0.041 Uiso 1 1 calc R U . . .
C6 C 0.2217(8) 0.5503(5) 0.0683(5) 0.0415(18) Uani 1 1 d . U . . .
H6A H 0.1701 0.5427 0.0130 0.062 Uiso 1 1 calc R U . . .
H6B H 0.2660 0.6188 0.0749 0.062 Uiso 1 1 calc R U . . .
H6C H 0.1529 0.5420 0.1066 0.062 Uiso 1 1 calc R U . . .
C7 C 0.5154(7) 0.3733(5) 0.1817(4) 0.0328(14) Uani 1 1 d . U . . .
H7A H 0.5723 0.3770 0.2366 0.039 Uiso 1 1 calc R U . . .
H7B H 0.4520 0.3119 0.1798 0.039 Uiso 1 1 calc R U . . .
C8 C 0.6203(8) 0.3576(6) 0.1222(5) 0.0457(19) Uani 1 1 d . U . . .
H8A H 0.5662 0.3556 0.0672 0.069 Uiso 1 1 calc R U . . .
H8B H 0.6725 0.2926 0.1340 0.069 Uiso 1 1 calc R U . . .
H8C H 0.6902 0.4145 0.1269 0.069 Uiso 1 1 calc R U . . .
C9 C 0.0405(7) 0.4608(5) 0.3569(5) 0.0341(15) Uani 1 1 d . U . . .
H9A H 0.0106 0.4695 0.4107 0.041 Uiso 1 1 calc R U . . .
H9B H 0.0084 0.3918 0.3367 0.041 Uiso 1 1 calc R U . . .
C10 C -0.0356(9) 0.5409(7) 0.3003(6) 0.058(2) Uani 1 1 d . U . . .
H10A H 0.0064 0.5415 0.2502 0.088 Uiso 1 1 calc R U . . .
H10B H -0.0232 0.6087 0.3259 0.088 Uiso 1 1 calc R U . . .
H10C H -0.1395 0.5246 0.2880 0.088 Uiso 1 1 calc R U . . .
C11 C 0.2650(7) 0.3738(5) 0.4160(4) 0.0325(13) Uani 1 1 d . U . . .
H11A H 0.2372 0.3108 0.3842 0.039 Uiso 1 1 calc R U . . .
H11B H 0.3724 0.3787 0.4237 0.039 Uiso 1 1 calc R U . . .
C12 C 0.2195(8) 0.3609(6) 0.4978(5) 0.0404(17) Uani 1 1 d . U . . .
H12A H 0.1133 0.3556 0.4916 0.061 Uiso 1 1 calc R U . . .
H12B H 0.2520 0.4205 0.5317 0.061 Uiso 1 1 calc R U . . .
H12C H 0.2635 0.2983 0.5234 0.061 Uiso 1 1 calc R U . . .
N2 N 0.4195(6) 0.4676(4) 0.1686(4) 0.0296(10) Uani 1 1 d . U . . .
N3 N 0.4060(6) 0.5852(4) 0.3047(3) 0.0320(11) Uani 1 1 d . U . . .
H3 H 0.3520 0.6481 0.2826 0.038 Uiso 1 1 calc R U . . .
N4 N 0.2028(6) 0.4660(4) 0.3661(3) 0.0261(9) Uani 1 1 d . U . . .
Pt1 Pt 0.29160(2) 0.46236(2) 0.26008(2) 0.02476(11) Uani 1 1 d . U . . .
N1 N 0.1858(3) 0.3299(4) 0.22010(14) 0.0369(10) Uani 0.324(9) 1 d D U P A 1
O1 O 0.2349(7) 0.2504(8) 0.2422(3) 0.064(2) Uani 0.324(9) 1 d D U P A 1
O2 O 0.0732(8) 0.3403(13) 0.1738(4) 0.064(2) Uani 0.324(9) 1 d D U P A 1
N1A N 0.0643(7) 0.3198(7) 0.1707(3) 0.0369(10) Uani 0.622(10) 1 d D U P A 2
O1A O 0.1858(3) 0.3299(4) 0.22010(14) 0.0369(10) Uani 0.622(10) 1 d D U P A 2
O2A O 0.0142(7) 0.4084(6) 0.1480(4) 0.064(2) Uani 0.622(10) 1 d D U P A 2
O1B O 0.1858(3) 0.3299(4) 0.22010(14) 0.0369(10) Uani 0.054(10) 1 d D U P A 3
N1B N 0.0727(14) 0.366(3) 0.1729(6) 0.0369(10) Uani 0.054(10) 1 d D U P A 3
O2B O -0.0059(15) 0.289(4) 0.1428(7) 0.064(2) Uani 0.054(10) 1 d D U P A 3
C13 C 0.6087(7) 0.1978(5) 0.4040(4) 0.0304(9) Uani 1 1 d . U . . .
F1 F 0.6543(4) 0.1003(3) 0.4006(3) 0.0383(9) Uani 1 1 d . U . . .
F2 F 0.4945(4) 0.2098(3) 0.3449(2) 0.0377(9) Uani 1 1 d . U . . .
F3 F 0.5599(4) 0.2090(3) 0.4743(3) 0.0418(9) Uani 1 1 d . U . . .
O3 O 0.7896(5) 0.2631(4) 0.3153(3) 0.0388(11) Uani 1 1 d . U . . .
O4 O 0.6814(5) 0.3865(4) 0.3967(3) 0.0374(11) Uani 1 1 d . U . . .
O5 O 0.8606(5) 0.2645(4) 0.4613(3) 0.0447(12) Uani 1 1 d . U . . .
S1 S 0.75232(17) 0.28827(12) 0.39328(11) 0.0306(4) Uani 1 1 d . 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
C1 N2 1.504(8) . ?
C1 C2 1.519(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.486(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.479(9) . ?
C3 C4 1.503(10) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.504(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.480(9) . ?
C5 C6 1.533(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.513(9) . ?
C7 N2 1.514(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.496(8) . ?
C9 C10 1.510(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.505(9) . ?
C11 N4 1.524(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.083(6) . ?
N3 Pt1 2.001(5) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.073(5) . ?
Pt1 O1B 2.046(4) . ?
Pt1 O1A 2.046(4) . ?
Pt1 N1 2.046(4) . ?
N1 O1 1.167(8) . ?
N1 O2 1.210(8) . ?
N1A O2A 1.279(8) . ?
N1A O1A 1.300(7) . ?
O1B N1B 1.303(10) . ?
N1B O2B 1.299(10) . ?
C13 F3 1.335(8) . ?
C13 F1 1.341(7) . ?
C13 F2 1.345(8) . ?
C13 S1 1.811(6) . ?
O3 S1 1.441(5) . ?
O4 S1 1.444(5) . ?
O5 S1 1.433(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 111.5(5) . . ?
N2 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N2 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 105.0(5) . . ?
N3 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
N3 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
N3 C3 C4 106.7(6) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C3 C4 N4 109.7(6) . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
N4 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.3(6) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N2 116.1(6) . . ?
C8 C7 H7A 108.3 . . ?
N2 C7 H7A 108.3 . . ?
C8 C7 H7B 108.3 . . ?
N2 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.6(6) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 116.8(5) . . ?
C12 C11 H11A 108.1 . . ?
N4 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
N4 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 110.6(5) . . ?
C5 N2 C7 109.6(5) . . ?
C1 N2 C7 109.6(5) . . ?
C5 N2 Pt1 116.3(4) . . ?
C1 N2 Pt1 105.4(4) . . ?
C7 N2 Pt1 105.0(4) . . ?
C3 N3 C2 116.9(6) . . ?
C3 N3 Pt1 107.6(4) . . ?
C2 N3 Pt1 108.4(4) . . ?
C3 N3 H3 107.9 . . ?
C2 N3 H3 107.9 . . ?
Pt1 N3 H3 107.9 . . ?
C9 N4 C4 110.5(5) . . ?
C9 N4 C11 108.2(5) . . ?
C4 N4 C11 109.8(6) . . ?
C9 N4 Pt1 116.2(5) . . ?
C4 N4 Pt1 105.5(4) . . ?
C11 N4 Pt1 106.5(4) . . ?
N3 Pt1 O1B 175.6(2) . . ?
N3 Pt1 O1A 175.6(2) . . ?
N3 Pt1 N1 175.6(2) . . ?
N3 Pt1 N4 85.5(2) . . ?
O1B Pt1 N4 93.69(15) . . ?
O1A Pt1 N4 93.69(15) . . ?
N1 Pt1 N4 93.69(15) . . ?
N3 Pt1 N2 85.3(2) . . ?
O1B Pt1 N2 95.02(16) . . ?
O1A Pt1 N2 95.02(16) . . ?
N1 Pt1 N2 95.02(16) . . ?
N4 Pt1 N2 168.4(2) . . ?
O1 N1 O2 124.1(9) . . ?
O1 N1 Pt1 119.8(5) . . ?
O2 N1 Pt1 116.1(9) . . ?
O2A N1A O1A 109.8(7) . . ?
N1A O1A Pt1 128.4(5) . . ?
N1B O1B Pt1 101.3(17) . . ?
O2B N1B O1B 107.9(11) . . ?
F3 C13 F1 107.1(5) . . ?
F3 C13 F2 107.4(5) . . ?
F1 C13 F2 107.3(5) . . ?
F3 C13 S1 112.0(4) . . ?
F1 C13 S1 111.6(4) . . ?
F2 C13 S1 111.2(5) . . ?
O5 S1 O3 115.7(3) . . ?
O5 S1 O4 115.4(3) . . ?
O3 S1 O4 114.4(3) . . ?
O5 S1 C13 102.7(3) . . ?
O3 S1 C13 103.1(3) . . ?
O4 S1 C13 102.9(3) . . ?

_refine_diff_density_max         2.017
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.189

####################################################################### 
# 
# 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_VT_120K
_database_code_depnum_ccdc_archive 'CCDC 1564451'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2689(4)
_cell_length_b                   13.0528(5)
_cell_length_c                   16.7054(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.782(4)
_cell_angle_gamma                90
_cell_volume                     1997.41(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3597
_cell_measurement_theta_min      3.9930
_cell_measurement_theta_max      28.8140

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.092
_shelx_estimated_absorpt_T_min   0.639
_shelx_estimated_absorpt_T_max   0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8852
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.357
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4069
_reflns_number_gt                3351
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0279P)²+1.1341P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4069
_refine_ls_number_parameters     270
_refine_ls_number_restraints     243
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0716
_refine_ls_wR_factor_gt          0.0661
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.032
_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 0.2576(4) 0.4373(2) 0.40867(19) 0.0249(7) Uani 1 1 d . U . . .
H1A H 0.2554 0.4427 0.4676 0.030 Uiso 1 1 calc R U . . .
H1B H 0.1931 0.3800 0.3872 0.030 Uiso 1 1 calc R U . . .
C2 C 0.4108(4) 0.4160(3) 0.39430(18) 0.0255(7) Uani 1 1 d . U . . .
H2A H 0.4781 0.4699 0.4194 0.031 Uiso 1 1 calc R U . . .
H2B H 0.4446 0.3489 0.4178 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5488(3) 0.4174(3) 0.27537(18) 0.0250(7) Uani 1 1 d . U . . .
H3A H 0.5999 0.3510 0.2858 0.030 Uiso 1 1 calc R U . . .
H3B H 0.6115 0.4723 0.3027 0.030 Uiso 1 1 calc R U . . .
C4 C 0.5143(4) 0.4377(2) 0.18496(18) 0.0246(7) Uani 1 1 d . U . . .
H4A H 0.6063 0.4460 0.1623 0.030 Uiso 1 1 calc R U . . .
H4B H 0.4605 0.3787 0.1577 0.030 Uiso 1 1 calc R U . . .
C5 C 0.0404(3) 0.5412(3) 0.35678(19) 0.0252(7) Uani 1 1 d . U . . .
H5A H 0.0094 0.6104 0.3369 0.030 Uiso 1 1 calc R U . . .
H5B H 0.0085 0.5319 0.4102 0.030 Uiso 1 1 calc R U . . .
C6 C -0.0357(4) 0.4625(3) 0.2987(2) 0.0423(9) Uani 1 1 d . U . . .
H6A H 0.0077 0.4626 0.2487 0.064 Uiso 1 1 calc R U . . .
H6B H -0.1397 0.4794 0.2859 0.064 Uiso 1 1 calc R U . . .
H6C H -0.0245 0.3945 0.3237 0.064 Uiso 1 1 calc R U . . .
C7 C 0.2674(4) 0.6264(2) 0.41534(18) 0.0239(6) Uani 1 1 d . U . . .
H7A H 0.2408 0.6889 0.3828 0.029 Uiso 1 1 calc R U . . .
H7B H 0.3750 0.6201 0.4228 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2216(4) 0.6414(3) 0.49824(19) 0.0303(8) Uani 1 1 d . U . . .
H8A H 0.1170 0.6570 0.4917 0.046 Uiso 1 1 calc R U . . .
H8B H 0.2769 0.6984 0.5262 0.046 Uiso 1 1 calc R U . . .
H8C H 0.2414 0.5787 0.5302 0.046 Uiso 1 1 calc R U . . .
C9 C 0.3420(4) 0.5327(2) 0.08467(18) 0.0250(7) Uani 1 1 d . U . . .
H9A H 0.4123 0.5211 0.0465 0.030 Uiso 1 1 calc R U . . .
H9B H 0.2973 0.6009 0.0726 0.030 Uiso 1 1 calc R U . . .
C10 C 0.2240(4) 0.4522(3) 0.0703(2) 0.0309(8) Uani 1 1 d . U . . .
H10A H 0.1693 0.4602 0.0156 0.046 Uiso 1 1 calc R U . . .
H10B H 0.1575 0.4602 0.1102 0.046 Uiso 1 1 calc R U . . .
H10C H 0.2685 0.3839 0.0757 0.046 Uiso 1 1 calc R U . . .
C11 C 0.5179(4) 0.6275(2) 0.18295(18) 0.0245(7) Uani 1 1 d . U . . .
H11A H 0.5731 0.6243 0.2385 0.029 Uiso 1 1 calc R U . . .
H11B H 0.4533 0.6881 0.1802 0.029 Uiso 1 1 calc R U . . .
C12 C 0.6260(4) 0.6438(3) 0.1246(2) 0.0332(8) Uani 1 1 d . U . . .
H12A H 0.5728 0.6556 0.0700 0.050 Uiso 1 1 calc R U . . .
H12B H 0.6878 0.5830 0.1243 0.050 Uiso 1 1 calc R U . . .
H12C H 0.6871 0.7035 0.1417 0.050 Uiso 1 1 calc R U . . .
N2 N 0.2030(3) 0.53566(19) 0.36750(14) 0.0189(5) Uani 1 1 d . U . . .
N3 N 0.4059(3) 0.4151(2) 0.30503(14) 0.0212(5) Uani 1 1 d . U . . .
H3 H 0.3519 0.3525 0.2829 0.025 Uiso 1 1 calc R U . . .
N4 N 0.4234(3) 0.53320(18) 0.16934(14) 0.0191(5) Uani 1 1 d . U . . .
Pd1 Pd 0.29232(2) 0.53847(2) 0.26025(2) 0.01736(8) Uani 1 1 d . U . . .
N1_a N 0.1880(16) 0.6633(9) 0.2185(9) 0.023(2) Uani 0.433(7) 1 d D U P A 1
O1_a O 0.2339(7) 0.7448(5) 0.2468(4) 0.0425(18) Uani 0.433(7) 1 d D U P A 1
O2_a O 0.0779(13) 0.6599(7) 0.1675(8) 0.0425(18) Uani 0.433(7) 1 d D U P A 1
N1A_b N 0.0651(9) 0.6801(5) 0.1719(6) 0.0263(16) Uani 0.567(7) 1 d D U P A 2
O1A_b O 0.1889(9) 0.6761(6) 0.2206(6) 0.0194(15) Uani 0.567(7) 1 d D U P A 2
O2A_b O 0.0159(5) 0.5929(3) 0.1526(3) 0.0360(14) Uani 0.567(7) 1 d D U P A 2
C13 C 0.6079(3) 0.8043(2) 0.40441(19) 0.0226(5) Uani 1 1 d . U . . .
F1 F 0.6552(2) 0.90107(13) 0.40109(11) 0.0298(4) Uani 1 1 d . U . . .
F2 F 0.5587(2) 0.79372(15) 0.47517(11) 0.0331(5) Uani 1 1 d . U . . .
F3 F 0.4945(2) 0.79329(14) 0.34544(11) 0.0304(4) Uani 1 1 d . U . . .
O3 O 0.7912(3) 0.73771(17) 0.31662(13) 0.0299(5) Uani 1 1 d . U . . .
O4 O 0.6777(2) 0.61549(17) 0.39703(13) 0.0272(5) Uani 1 1 d . U . . .
O5 O 0.8594(2) 0.73441(18) 0.46340(14) 0.0327(6) Uani 1 1 d . U . . .
S1 S 0.75162(8) 0.71295(6) 0.39427(5) 0.02185(17) Uani 1 1 d . 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
C1 C2 1.502(4) . ?
C1 N2 1.507(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.485(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.484(4) . ?
C3 C4 1.519(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.504(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.492(4) . ?
C5 C6 1.512(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.500(4) . ?
C7 C8 1.522(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.498(4) . ?
C9 C10 1.509(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.507(4) . ?
C11 C12 1.516(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pd1 2.086(2) . ?
N3 Pd1 2.005(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.086(2) . ?
Pd1 N1_a 1.967(14) . ?
Pd1 O1A_b 2.095(8) . ?
N1_a O1_a 1.214(9) . ?
N1_a O2_a 1.226(8) . ?
N1A_b O2A_b 1.251(7) . ?
N1A_b O1A_b 1.303(6) . ?
C13 F3 1.334(3) . ?
C13 F2 1.337(3) . ?
C13 F1 1.341(4) . ?
C13 S1 1.815(3) . ?
O3 S1 1.438(2) . ?
O4 S1 1.449(2) . ?
O5 S1 1.435(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 N2 110.2(2) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.1(3) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.8(2) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.2(2) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 114.1(3) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 116.3(3) . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7B 108.2 . . ?
C8 C7 H7B 108.2 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.7(3) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.4(3) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C7 109.7(2) . . ?
C5 N2 C1 111.0(2) . . ?
C7 N2 C1 110.6(2) . . ?
C5 N2 Pd1 114.96(19) . . ?
C7 N2 Pd1 105.43(17) . . ?
C1 N2 Pd1 104.91(17) . . ?
C3 N3 C2 116.3(2) . . ?
C3 N3 Pd1 107.73(18) . . ?
C2 N3 Pd1 107.63(19) . . ?
C3 N3 H3 108.3 . . ?
C2 N3 H3 108.3 . . ?
Pd1 N3 H3 108.3 . . ?
C9 N4 C4 110.4(2) . . ?
C9 N4 C11 110.1(2) . . ?
C4 N4 C11 110.7(2) . . ?
C9 N4 Pd1 114.98(19) . . ?
C4 N4 Pd1 105.90(17) . . ?
C11 N4 Pd1 104.66(17) . . ?
N1_a Pd1 N3 177.5(3) . . ?
N1_a Pd1 N2 94.6(5) . . ?
N3 Pd1 N2 85.41(10) . . ?
N1_a Pd1 N4 94.5(5) . . ?
N3 Pd1 N4 85.07(10) . . ?
N2 Pd1 N4 167.58(10) . . ?
N3 Pd1 O1A_b 174.4(2) . . ?
N2 Pd1 O1A_b 93.7(3) . . ?
N4 Pd1 O1A_b 95.0(3) . . ?
O1_a N1_a O2_a 120.5(13) . . ?
O1_a N1_a Pd1 117.6(10) . . ?
O2_a N1_a Pd1 121.9(8) . . ?
O2A_b N1A_b O1A_b 112.1(6) . . ?
N1A_b O1A_b Pd1 123.3(5) . . ?
F3 C13 F2 107.8(2) . . ?
F3 C13 F1 107.3(2) . . ?
F2 C13 F1 106.9(2) . . ?
F3 C13 S1 111.5(2) . . ?
F2 C13 S1 111.6(2) . . ?
F1 C13 S1 111.4(2) . . ?
O5 S1 O3 116.10(15) . . ?
O5 S1 O4 114.87(14) . . ?
O3 S1 O4 114.39(13) . . ?
O5 S1 C13 103.17(14) . . ?
O3 S1 C13 103.21(14) . . ?
O4 S1 C13 102.50(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 -56.0(3) . . . . ?
N3 C3 C4 N4 54.5(3) . . . . ?
C6 C5 N2 C7 171.1(3) . . . . ?
C6 C5 N2 C1 -66.4(3) . . . . ?
C6 C5 N2 Pd1 52.5(3) . . . . ?
C8 C7 N2 C5 56.7(3) . . . . ?
C8 C7 N2 C1 -66.1(3) . . . . ?
C8 C7 N2 Pd1 -179.0(2) . . . . ?
C2 C1 N2 C5 161.0(3) . . . . ?
C2 C1 N2 C7 -77.0(3) . . . . ?
C2 C1 N2 Pd1 36.2(3) . . . . ?
C4 C3 N3 C2 -168.8(3) . . . . ?
C4 C3 N3 Pd1 -48.0(3) . . . . ?
C1 C2 N3 C3 167.6(3) . . . . ?
C1 C2 N3 Pd1 46.7(3) . . . . ?
C10 C9 N4 C4 68.4(3) . . . . ?
C10 C9 N4 C11 -169.1(3) . . . . ?
C10 C9 N4 Pd1 -51.3(3) . . . . ?
C3 C4 N4 C9 -158.3(3) . . . . ?
C3 C4 N4 C11 79.6(3) . . . . ?
C3 C4 N4 Pd1 -33.2(3) . . . . ?
C12 C11 N4 C9 -55.8(4) . . . . ?
C12 C11 N4 C4 66.4(3) . . . . ?
C12 C11 N4 Pd1 -179.9(2) . . . . ?
O2A_b N1A_b O1A_b Pd1 0.5(10) . . . . ?
F3 C13 S1 O5 -178.2(2) . . . . ?
F2 C13 S1 O5 -57.5(2) . . . . ?
F1 C13 S1 O5 62.0(2) . . . . ?
F3 C13 S1 O3 60.5(2) . . . . ?
F2 C13 S1 O3 -178.8(2) . . . . ?
F1 C13 S1 O3 -59.3(2) . . . . ?
F3 C13 S1 O4 -58.6(2) . . . . ?
F2 C13 S1 O4 62.1(2) . . . . ?
F1 C13 S1 O4 -178.4(2) . . . . ?

_refine_diff_density_max         0.618
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.091

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_Pt_VT_220K
_database_code_depnum_ccdc_archive 'CCDC 1564475'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3358(2)
_cell_length_b                   12.9883(3)
_cell_length_c                   16.7838(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.045(3)
_cell_angle_gamma                90
_cell_volume                     2009.83(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    9584
_cell_measurement_theta_min      3.9700
_cell_measurement_theta_max      29.5810

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 5 0.1067
0 3 -5 0.1696
-3 5 2 0.1520
-3 -5 2 0.1832
-5 1 4 0.0508
0 -1 1 0.1437
-1 0 -5 0.1033
-1 -5 -3 0.2517
-1 1 -5 0.1103
1 5 -1 0.2318
-5 0 4 0.0512
5 0 -4 0.0348
_exptl_absorpt_coefficient_mu    7.144
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            22004
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.369
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4103
_reflns_number_gt                3628
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0185P)²+1.2200P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4103
_refine_ls_number_parameters     255
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0446
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.002
_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 -0.0079(4) 0.5634(3) 0.8168(2) 0.0325(7) Uani 1 1 d . U . . .
H1A H -0.0980 0.5545 0.8392 0.039 Uiso 1 1 calc R U . . .
H1B H 0.0446 0.6222 0.8439 0.039 Uiso 1 1 calc R U . . .
C2 C -0.0433(4) 0.5843(3) 0.7277(2) 0.0322(7) Uani 1 1 d . U . . .
H2A H -0.1051 0.5296 0.7007 0.039 Uiso 1 1 calc R U . . .
H2B H -0.0940 0.6502 0.7178 0.039 Uiso 1 1 calc R U . . .
C3 C 0.0893(4) 0.5847(3) 0.60802(19) 0.0336(7) Uani 1 1 d . U . . .
H3A H 0.0537 0.6506 0.5843 0.040 Uiso 1 1 calc R U . . .
H3B H 0.0239 0.5299 0.5846 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2416(4) 0.5646(3) 0.5927(2) 0.0347(7) Uani 1 1 d . U . . .
H4A H 0.2422 0.5582 0.5346 0.042 Uiso 1 1 calc R U . . .
H4B H 0.3044 0.6225 0.6129 0.042 Uiso 1 1 calc R U . . .
C5 C -0.0098(4) 0.3726(2) 0.8190(2) 0.0325(7) Uani 1 1 d . U . . .
H5A H 0.0540 0.3123 0.8224 0.039 Uiso 1 1 calc R U . . .
H5B H -0.0639 0.3749 0.7641 0.039 Uiso 1 1 calc R U . . .
C6 C -0.1177(4) 0.3569(3) 0.8771(2) 0.0483(10) Uani 1 1 d . U . . .
H6A H -0.1784 0.2978 0.8601 0.072 Uiso 1 1 calc R U . . .
H6B H -0.1779 0.4178 0.8772 0.072 Uiso 1 1 calc R U . . .
H6C H -0.0656 0.3451 0.9310 0.072 Uiso 1 1 calc R U . . .
C7 C 0.1648(4) 0.4680(3) 0.9169(2) 0.0346(7) Uani 1 1 d . U . . .
H7A H 0.2124 0.4011 0.9280 0.042 Uiso 1 1 calc R U . . .
H7B H 0.0950 0.4763 0.9544 0.042 Uiso 1 1 calc R U . . .
C8 C 0.2779(4) 0.5520(3) 0.9330(2) 0.0426(9) Uani 1 1 d . U . . .
H8A H 0.3420 0.5487 0.8929 0.064 Uiso 1 1 calc R U . . .
H8B H 0.3339 0.5425 0.9863 0.064 Uiso 1 1 calc R U . . .
H8C H 0.2304 0.6186 0.9302 0.064 Uiso 1 1 calc R U . . .
C9 C 0.2369(4) 0.3744(2) 0.5869(2) 0.0328(7) Uani 1 1 d . U . . .
H9A H 0.1308 0.3787 0.5800 0.039 Uiso 1 1 calc R U . . .
H9B H 0.2658 0.3127 0.6191 0.039 Uiso 1 1 calc R U . . .
C10 C 0.2808(4) 0.3598(3) 0.5040(2) 0.0422(9) Uani 1 1 d . U . . .
H10A H 0.2524 0.4199 0.4710 0.063 Uiso 1 1 calc R U . . .
H10B H 0.2330 0.2993 0.4785 0.063 Uiso 1 1 calc R U . . .
H10C H 0.3851 0.3509 0.5098 0.063 Uiso 1 1 calc R U . . .
C11 C 0.4610(4) 0.4636(3) 0.6438(2) 0.0377(8) Uani 1 1 d . U . . .
H11A H 0.4897 0.4696 0.5903 0.045 Uiso 1 1 calc R U . . .
H11B H 0.4946 0.3966 0.6662 0.045 Uiso 1 1 calc R U . . .
C12 C 0.5356(5) 0.5470(3) 0.6972(3) 0.0557(11) Uani 1 1 d . U . . .
H12A H 0.5216 0.6127 0.6696 0.084 Uiso 1 1 calc R U . . .
H12B H 0.6385 0.5321 0.7096 0.084 Uiso 1 1 calc R U . . .
H12C H 0.4949 0.5501 0.7469 0.084 Uiso 1 1 calc R U . . .
N2 N 0.0838(3) 0.46756(18) 0.83202(16) 0.0256(5) Uani 1 1 d . U . . .
N3 N 0.0977(3) 0.5873(2) 0.69727(15) 0.0264(5) Uani 1 1 d . U . . .
H3 H 0.1508 0.6500 0.7183 0.032 Uiso 1 1 calc R U . . .
N4 N 0.2982(3) 0.46699(18) 0.63475(16) 0.0264(5) Uani 1 1 d . U . . .
Pt1 Pt 0.21196(2) 0.46362(2) 0.74133(2) 0.02144(5) Uani 1 1 d . U . . .
N1 N 0.3123(2) 0.32835(17) 0.77930(14) 0.0333(5) Uani 0.090(4) 1 d D U P A 1
O1 O 0.276(2) 0.2475(11) 0.7508(13) 0.0333(5) Uani 0.090(4) 1 d D U P A 1
O2 O 0.414(3) 0.338(2) 0.8333(17) 0.0333(5) Uani 0.090(4) 1 d D U P A 1
N1A N 0.4386(4) 0.3226(3) 0.8277(3) 0.0465(11) Uani 0.910(4) 1 d D U P A 2
O1A O 0.3123(2) 0.32835(17) 0.77930(14) 0.0333(5) Uani 0.910(4) 1 d D U P A 2
O2A O 0.4888(3) 0.4056(2) 0.8489(2) 0.0620(10) Uani 0.910(4) 1 d D U P A 2
C13 C 0.6088(4) 0.6999(3) 0.9033(2) 0.0324(6) Uani 1 1 d . U . . .
F1 F 0.6536(2) 0.60263(15) 0.89966(13) 0.0463(5) Uani 1 1 d . U . . .
F2 F 0.5606(2) 0.71135(16) 0.97323(13) 0.0508(5) Uani 1 1 d . U . . .
F3 F 0.4954(2) 0.71199(15) 0.84477(13) 0.0458(5) Uani 1 1 d . U . . .
O3 O 0.8601(3) 0.7667(2) 0.96101(17) 0.0520(7) Uani 1 1 d . U . . .
O4 O 0.6824(3) 0.88829(18) 0.89598(15) 0.0411(6) Uani 1 1 d . U . . .
O5 O 0.7894(3) 0.7647(2) 0.81532(16) 0.0471(6) Uani 1 1 d . U . . .
S1 S 0.75266(9) 0.78972(6) 0.89264(5) 0.03188(18) Uani 1 1 d . 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
C1 C2 1.505(5) . ?
C1 N2 1.510(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.485(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.488(4) . ?
C3 C4 1.507(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.506(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.507(4) . ?
C5 C6 1.522(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N2 1.505(4) . ?
C7 C8 1.513(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N4 1.507(4) . ?
C9 C10 1.523(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 N4 1.504(4) . ?
C11 C12 1.505(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
N2 Pt1 2.079(3) . ?
N3 Pt1 2.004(2) . ?
N3 H3 0.9900 . ?
N4 Pt1 2.075(3) . ?
Pt1 O1A 2.045(2) . ?
Pt1 N1 2.045(2) . ?
N1 O1 1.180(9) . ?
N1 O2 1.211(10) . ?
N1A O2A 1.206(5) . ?
N1A O1A 1.325(4) . ?
C13 F2 1.330(4) . ?
C13 F3 1.335(4) . ?
C13 F1 1.335(4) . ?
C13 S1 1.809(3) . ?
O3 S1 1.432(3) . ?
O4 S1 1.443(2) . ?
O5 S1 1.431(3) . ?

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 N2 110.3(3) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.2(3) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.9(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 109.7(3) . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 116.4(3) . . ?
N2 C5 H5A 108.2 . . ?
C6 C5 H5A 108.2 . . ?
N2 C5 H5B 108.2 . . ?
C6 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 113.9(3) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 116.8(3) . . ?
N4 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N4 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 113.9(3) . . ?
N4 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N4 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 N2 C5 109.5(2) . . ?
C7 N2 C1 110.1(2) . . ?
C5 N2 C1 110.4(3) . . ?
C7 N2 Pt1 115.6(2) . . ?
C5 N2 Pt1 105.14(18) . . ?
C1 N2 Pt1 105.83(18) . . ?
C2 N3 C3 115.9(3) . . ?
C2 N3 Pt1 107.53(19) . . ?
C3 N3 Pt1 107.11(18) . . ?
C2 N3 H3 108.7 . . ?
C3 N3 H3 108.7 . . ?
Pt1 N3 H3 108.7 . . ?
C11 N4 C4 110.3(3) . . ?
C11 N4 C9 108.9(2) . . ?
C4 N4 C9 110.3(3) . . ?
C11 N4 Pt1 115.8(2) . . ?
C4 N4 Pt1 105.45(18) . . ?
C9 N4 Pt1 106.00(19) . . ?
N3 Pt1 O1A 174.03(10) . . ?
N3 Pt1 N1 174.03(10) . . ?
N3 Pt1 N4 85.49(10) . . ?
O1A Pt1 N4 93.78(9) . . ?
N1 Pt1 N4 93.78(9) . . ?
N3 Pt1 N2 85.19(10) . . ?
O1A Pt1 N2 94.64(9) . . ?
N1 Pt1 N2 94.64(9) . . ?
N4 Pt1 N2 167.63(10) . . ?
O1 N1 O2 122.6(13) . . ?
O1 N1 Pt1 123.4(11) . . ?
O2 N1 Pt1 114.0(14) . . ?
O2A N1A O1A 113.5(4) . . ?
N1A O1A Pt1 124.0(2) . . ?
F2 C13 F3 107.3(3) . . ?
F2 C13 F1 107.4(3) . . ?
F3 C13 F1 107.2(3) . . ?
F2 C13 S1 112.0(2) . . ?
F3 C13 S1 111.5(2) . . ?
F1 C13 S1 111.3(2) . . ?
O5 S1 O3 116.23(17) . . ?
O5 S1 O4 114.30(16) . . ?
O3 S1 O4 114.79(16) . . ?
O5 S1 C13 103.36(16) . . ?
O3 S1 C13 102.92(16) . . ?
O4 S1 C13 102.66(16) . . ?

_refine_diff_density_max         0.784
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_Pt_VT_110K
_database_code_depnum_ccdc_archive 'CCDC 1564466'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_Pt_VT_110K          
;
PROBLEM: Check Calcd Positive Residual Density on     Pt1       1.68 eA-3
RESPONSE: The residual density around the heavy Pt1 atom may be the result of fourier transform termination ripples, resulting from slightly reduced diffraction quality following a long period of photo-irradiation with this crystal (< 3 hrs).
;
# Added during the CSD deposition process: Tuesday 25 July 2017 11:25 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3083(4)
_cell_length_b                   13.0063(5)
_cell_length_c                   16.7422(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.957(4)
_cell_angle_gamma                90
_cell_volume                     2002.20(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    3268
_cell_measurement_theta_min      3.8110
_cell_measurement_theta_max      29.2810

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.171
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9268
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.366
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4088
_reflns_number_gt                3294
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0454P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4088
_refine_ls_number_parameters     257
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0900
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.015
_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 0.5114(7) 0.5628(5) 0.1843(4) 0.0319(13) Uani 1 1 d . U . . .
H1A H 0.6026 0.5534 0.1617 0.038 Uiso 1 1 calc R U . . .
H1B H 0.4590 0.6224 0.1569 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5474(7) 0.5844(5) 0.2737(4) 0.0310(13) Uani 1 1 d . U . . .
H2A H 0.6114 0.5300 0.3011 0.037 Uiso 1 1 calc R U . . .
H2B H 0.5974 0.6514 0.2833 0.037 Uiso 1 1 calc R U . . .
C3 C 0.4116(7) 0.5851(5) 0.3930(4) 0.0341(14) Uani 1 1 d . U . . .
H3A H 0.4460 0.6523 0.4163 0.041 Uiso 1 1 calc R U . . .
H3B H 0.4788 0.5309 0.4178 0.041 Uiso 1 1 calc R U . . .
C4 C 0.2588(7) 0.5639(5) 0.4086(4) 0.0317(13) Uani 1 1 d . U . . .
H4A H 0.2583 0.5575 0.4674 0.038 Uiso 1 1 calc R U . . .
H4B H 0.1943 0.6217 0.3880 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3396(7) 0.4689(5) 0.0842(4) 0.0310(13) Uani 1 1 d . U . . .
H5A H 0.2948 0.4006 0.0716 0.037 Uiso 1 1 calc R U . . .
H5B H 0.4106 0.4806 0.0469 0.037 Uiso 1 1 calc R U . . .
C6 C 0.2212(8) 0.5510(5) 0.0689(5) 0.0412(17) Uani 1 1 d . U . . .
H6A H 0.1756 0.5486 0.0120 0.062 Uiso 1 1 calc R U . . .
H6B H 0.2644 0.6190 0.0811 0.062 Uiso 1 1 calc R U . . .
H6C H 0.1475 0.5380 0.1036 0.062 Uiso 1 1 calc R U . . .
C7 C 0.5150(7) 0.3728(5) 0.1811(4) 0.0336(13) Uani 1 1 d . U . . .
H7A H 0.5714 0.3763 0.2363 0.040 Uiso 1 1 calc R U . . .
H7B H 0.4515 0.3116 0.1790 0.040 Uiso 1 1 calc R U . . .
C8 C 0.6208(7) 0.3566(6) 0.1223(4) 0.0416(17) Uani 1 1 d . U . . .
H8A H 0.5672 0.3526 0.0672 0.062 Uiso 1 1 calc R U . . .
H8B H 0.6746 0.2925 0.1355 0.062 Uiso 1 1 calc R U . . .
H8C H 0.6892 0.4144 0.1261 0.062 Uiso 1 1 calc R U . . .
C9 C 0.0402(7) 0.4619(5) 0.3571(4) 0.0330(14) Uani 1 1 d . U . . .
H9A H 0.0074 0.3929 0.3371 0.040 Uiso 1 1 calc R U . . .
H9B H 0.0104 0.4712 0.4109 0.040 Uiso 1 1 calc R U . . .
C10 C -0.0353(9) 0.5411(6) 0.3006(5) 0.053(2) Uani 1 1 d . U . . .
H10A H 0.0089 0.5430 0.2512 0.079 Uiso 1 1 calc R U . . .
H10B H -0.0256 0.6087 0.3268 0.079 Uiso 1 1 calc R U . . .
H10C H -0.1385 0.5234 0.2869 0.079 Uiso 1 1 calc R U . . .
C11 C 0.2653(6) 0.3743(5) 0.4160(4) 0.0295(12) Uani 1 1 d . U . . .
H11A H 0.2373 0.3115 0.3839 0.035 Uiso 1 1 calc R U . . .
H11B H 0.3727 0.3790 0.4236 0.035 Uiso 1 1 calc R U . . .
C12 C 0.2202(7) 0.3605(6) 0.4977(4) 0.0404(16) Uani 1 1 d . U . . .
H12A H 0.1145 0.3515 0.4913 0.061 Uiso 1 1 calc R U . . .
H12B H 0.2483 0.4214 0.5309 0.061 Uiso 1 1 calc R U . . .
H12C H 0.2683 0.2997 0.5240 0.061 Uiso 1 1 calc R U . . .
N2 N 0.4185(6) 0.4676(4) 0.1684(3) 0.0278(9) Uani 1 1 d . U . . .
N3 N 0.4063(5) 0.5860(4) 0.3046(3) 0.0287(10) Uani 1 1 d . U . . .
H3 H 0.3520 0.6489 0.2828 0.034 Uiso 1 1 calc R U . . .
N4 N 0.2040(5) 0.4659(4) 0.3667(3) 0.0247(9) Uani 1 1 d . U . . .
Pt1 Pt 0.29148(2) 0.46268(2) 0.26002(2) 0.02327(10) Uani 1 1 d . U . . .
N1 N 0.1849(3) 0.3310(3) 0.21932(14) 0.0349(9) Uani 0.324(8) 1 d D U P A 1
O1 O 0.2345(7) 0.2512(8) 0.2409(3) 0.060(2) Uani 0.324(8) 1 d D U P A 1
O2 O 0.0715(8) 0.3411(12) 0.1732(4) 0.060(2) Uani 0.324(8) 1 d D U P A 1
N1A N 0.0624(7) 0.3203(7) 0.1699(3) 0.0349(9) Uani 0.572(9) 1 d D U P A 2
O1A O 0.1849(3) 0.3310(3) 0.21932(14) 0.0349(9) Uani 0.572(9) 1 d D U P A 2
O2A O 0.0109(7) 0.4080(6) 0.1474(4) 0.060(2) Uani 0.572(9) 1 d D U P A 2
O1B O 0.1849(3) 0.3310(3) 0.21932(14) 0.0349(9) Uani 0.104(9) 1 d D U P A 3
N1B N 0.0717(12) 0.3689(19) 0.1728(5) 0.0349(9) Uani 0.104(9) 1 d D U P A 3
O2B O -0.0085(12) 0.293(3) 0.1417(5) 0.060(2) Uani 0.104(9) 1 d D U P A 3
C13 C 0.6087(6) 0.1978(5) 0.4038(4) 0.0283(9) Uani 1 1 d . U . . .
F1 F 0.6540(4) 0.1008(3) 0.4000(2) 0.0354(8) Uani 1 1 d . U . . .
F2 F 0.4946(4) 0.2099(3) 0.3450(2) 0.0358(9) Uani 1 1 d . U . . .
F3 F 0.5594(4) 0.2092(3) 0.4739(2) 0.0406(9) Uani 1 1 d . U . . .
O3 O 0.7899(5) 0.2637(3) 0.3156(3) 0.0370(10) Uani 1 1 d . U . . .
O4 O 0.6811(5) 0.3871(3) 0.3965(3) 0.0342(10) Uani 1 1 d . U . . .
O5 O 0.8602(5) 0.2646(4) 0.4614(3) 0.0406(11) Uani 1 1 d . U . . .
S1 S 0.75226(16) 0.28835(11) 0.39303(10) 0.0287(4) Uani 1 1 d . 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
C1 C2 1.508(9) . ?
C1 N2 1.511(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.485(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.474(8) . ?
C3 C4 1.510(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.505(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.484(9) . ?
C5 C6 1.527(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.512(9) . ?
C7 N2 1.521(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.497(10) . ?
C9 N4 1.509(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.502(9) . ?
C11 N4 1.510(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.078(5) . ?
N3 Pt1 2.006(5) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.075(5) . ?
Pt1 O1B 2.042(4) . ?
Pt1 O1A 2.042(4) . ?
Pt1 N1 2.042(4) . ?
N1 O1 1.169(8) . ?
N1 O2 1.214(8) . ?
N1A O2A 1.272(8) . ?
N1A O1A 1.308(7) . ?
O1B N1B 1.306(10) . ?
N1B O2B 1.298(10) . ?
C13 F3 1.334(7) . ?
C13 F1 1.335(7) . ?
C13 F2 1.340(7) . ?
C13 S1 1.811(6) . ?
O3 S1 1.431(5) . ?
O4 S1 1.450(5) . ?
O5 S1 1.434(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 111.1(5) . . ?
C2 C1 H1A 109.4 . . ?
N2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 106.0(5) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.8(5) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 109.5(5) . . ?
N4 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N4 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 113.9(5) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N2 116.9(5) . . ?
C8 C7 H7A 108.1 . . ?
N2 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
N2 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N4 114.2(5) . . ?
C10 C9 H9A 108.7 . . ?
N4 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
N4 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 117.2(5) . . ?
C12 C11 H11A 108.0 . . ?
N4 C11 H11A 108.0 . . ?
C12 C11 H11B 108.0 . . ?
N4 C11 H11B 108.0 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 110.1(5) . . ?
C5 N2 C7 109.7(5) . . ?
C1 N2 C7 109.3(5) . . ?
C5 N2 Pt1 116.6(4) . . ?
C1 N2 Pt1 105.7(4) . . ?
C7 N2 Pt1 105.3(4) . . ?
C3 N3 C2 117.1(5) . . ?
C3 N3 Pt1 107.5(4) . . ?
C2 N3 Pt1 108.0(4) . . ?
C3 N3 H3 108.0 . . ?
C2 N3 H3 108.0 . . ?
Pt1 N3 H3 108.0 . . ?
C4 N4 C9 110.0(5) . . ?
C4 N4 C11 110.0(5) . . ?
C9 N4 C11 108.7(5) . . ?
C4 N4 Pt1 105.6(3) . . ?
C9 N4 Pt1 115.7(4) . . ?
C11 N4 Pt1 106.8(3) . . ?
N3 Pt1 O1B 176.10(18) . . ?
N3 Pt1 O1A 176.10(18) . . ?
N3 Pt1 N1 176.10(18) . . ?
N3 Pt1 N4 85.5(2) . . ?
O1B Pt1 N4 93.95(15) . . ?
O1A Pt1 N4 93.95(15) . . ?
N1 Pt1 N4 93.95(15) . . ?
N3 Pt1 N2 85.3(2) . . ?
O1B Pt1 N2 94.70(15) . . ?
O1A Pt1 N2 94.70(15) . . ?
N1 Pt1 N2 94.70(15) . . ?
N4 Pt1 N2 168.2(2) . . ?
O1 N1 O2 123.7(9) . . ?
O1 N1 Pt1 119.5(5) . . ?
O2 N1 Pt1 116.8(8) . . ?
O2A N1A O1A 110.1(7) . . ?
N1A O1A Pt1 129.1(5) . . ?
N1B O1B Pt1 100.8(12) . . ?
O2B N1B O1B 108.1(11) . . ?
F3 C13 F1 107.5(5) . . ?
F3 C13 F2 107.0(5) . . ?
F1 C13 F2 107.2(5) . . ?
F3 C13 S1 112.1(4) . . ?
F1 C13 S1 111.5(4) . . ?
F2 C13 S1 111.3(4) . . ?
O3 S1 O5 115.8(3) . . ?
O3 S1 O4 114.4(3) . . ?
O5 S1 O4 115.2(3) . . ?
O3 S1 C13 103.5(3) . . ?
O5 S1 C13 102.6(3) . . ?
O4 S1 C13 102.9(3) . . ?

_refine_diff_density_max         1.951
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.181

####################################################################### 
# 
# 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_VT_250K
_database_code_depnum_ccdc_archive 'CCDC 1564450'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N,N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2772(4)
_cell_length_b                   13.1359(6)
_cell_length_c                   17.2076(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.944(5)
_cell_angle_gamma                90
_cell_volume                     2085.72(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    2862
_cell_measurement_theta_min      3.8770
_cell_measurement_theta_max      29.1990

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.046
_shelx_estimated_absorpt_T_min   0.650
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9176
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.322
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4259
_reflns_number_gt                3294
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0260P)²+0.0406P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4259
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0723
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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 0.2582(4) 0.4381(2) 0.4071(2) 0.0416(9) Uani 1 1 d . . . . .
H1A H 0.1971 0.3830 0.3838 0.050 Uiso 1 1 calc R U . . .
H1B H 0.2478 0.4400 0.4632 0.050 Uiso 1 1 calc R U . . .
C2 C 0.4135(4) 0.4178(3) 0.3951(2) 0.0394(8) Uani 1 1 d . . . . .
H2A H 0.4769 0.4694 0.4218 0.047 Uiso 1 1 calc R U . . .
H2B H 0.4434 0.3506 0.4154 0.047 Uiso 1 1 calc R U . . .
C3 C 0.5660(3) 0.4253(2) 0.2822(2) 0.0392(9) Uani 1 1 d . . . . .
H3A H 0.6156 0.3599 0.2917 0.047 Uiso 1 1 calc R U . . .
H3B H 0.6253 0.4789 0.3090 0.047 Uiso 1 1 calc R U . . .
C4 C 0.5410(4) 0.4467(2) 0.1960(2) 0.0431(9) Uani 1 1 d . . . . .
H4A H 0.4913 0.3887 0.1694 0.052 Uiso 1 1 calc R U . . .
H4B H 0.6345 0.4554 0.1751 0.052 Uiso 1 1 calc R U . . .
C5 C 0.0482(3) 0.5427(3) 0.3582(2) 0.0526(10) Uani 1 1 d . . . . .
H5A H 0.0193 0.6127 0.3446 0.063 Uiso 1 1 calc R U . . .
H5B H 0.0091 0.5256 0.4074 0.063 Uiso 1 1 calc R U . . .
C6 C -0.0179(4) 0.4721(4) 0.2950(3) 0.0727(14) Uani 1 1 d . . . . .
H6A H 0.0254 0.4850 0.2470 0.109 Uiso 1 1 calc R U . . .
H6B H -0.1215 0.4840 0.2864 0.109 Uiso 1 1 calc R U . . .
H6C H 0.0000 0.4020 0.3110 0.109 Uiso 1 1 calc R U . . .
C7 C 0.2685(4) 0.6249(3) 0.4205(2) 0.0421(9) Uani 1 1 d . . . . .
H7A H 0.2443 0.6884 0.3922 0.051 Uiso 1 1 calc R U . . .
H7B H 0.3744 0.6194 0.4276 0.051 Uiso 1 1 calc R U . . .
C8 C 0.2140(4) 0.6325(3) 0.5007(2) 0.0590(11) Uani 1 1 d . . . . .
H8A H 0.1100 0.6435 0.4947 0.089 Uiso 1 1 calc R U . . .
H8B H 0.2613 0.6891 0.5292 0.089 Uiso 1 1 calc R U . . .
H8C H 0.2358 0.5698 0.5293 0.089 Uiso 1 1 calc R U . . .
C9 C 0.3772(4) 0.5389(3) 0.0994(2) 0.0500(10) Uani 1 1 d . . . . .
H9A H 0.4488 0.5224 0.0632 0.060 Uiso 1 1 calc R U . . .
H9B H 0.3389 0.6068 0.0859 0.060 Uiso 1 1 calc R U . . .
C10 C 0.2549(5) 0.4629(3) 0.0882(2) 0.0649(12) Uani 1 1 d . . . . .
H10A H 0.2136 0.4637 0.0341 0.097 Uiso 1 1 calc R U . . .
H10B H 0.1808 0.4808 0.1217 0.097 Uiso 1 1 calc R U . . .
H10C H 0.2917 0.3954 0.1017 0.097 Uiso 1 1 calc R U . . .
C11 C 0.5451(4) 0.6344(3) 0.1929(2) 0.0477(10) Uani 1 1 d . . . . .
H11A H 0.5940 0.6319 0.2462 0.057 Uiso 1 1 calc R U . . .
H11B H 0.4823 0.6945 0.1894 0.057 Uiso 1 1 calc R U . . .
C12 C 0.6594(5) 0.6480(3) 0.1365(3) 0.0770(15) Uani 1 1 d . . . . .
H12A H 0.6123 0.6566 0.0839 0.116 Uiso 1 1 calc R U . . .
H12B H 0.7214 0.5884 0.1384 0.116 Uiso 1 1 calc R U . . .
H12C H 0.7173 0.7077 0.1512 0.116 Uiso 1 1 calc R U . . .
N1 N 0.2030(3) 0.6712(2) 0.22720(18) 0.0404(7) Uani 1 1 d . . . . .
N2 N 0.2096(3) 0.53748(18) 0.37056(16) 0.0313(6) Uani 1 1 d . . . . .
N3 N 0.4208(3) 0.42235(18) 0.31029(15) 0.0279(6) Uani 1 1 d . . . . .
H3 H 0.3699 0.3617 0.2870 0.034 Uiso 1 1 calc R U . . .
N4 N 0.4511(3) 0.54130(18) 0.18029(16) 0.0348(6) Uani 1 1 d . . . . .
O1 O 0.2393(3) 0.7532(2) 0.2553(2) 0.0818(11) Uani 1 1 d . . . . .
O2 O 0.1017(4) 0.6691(2) 0.1777(2) 0.0972(12) Uani 1 1 d . . . . .
Pd1 Pd 0.31147(2) 0.54549(2) 0.26820(2) 0.02631(9) Uani 1 1 d . . . . .
C13 C 0.6114(4) 0.8130(3) 0.4146(2) 0.0475(9) Uani 1 1 d . . . . .
F1 F 0.6607(3) 0.90768(15) 0.41264(15) 0.0702(7) Uani 1 1 d . . . . .
F2 F 0.5555(3) 0.80196(18) 0.48130(15) 0.0766(8) Uani 1 1 d . . . . .
F3 F 0.5028(2) 0.80481(19) 0.35873(17) 0.0790(8) Uani 1 1 d . . . . .
O3 O 0.7939(3) 0.7433(2) 0.32694(17) 0.0647(8) Uani 1 1 d . . . . .
O4 O 0.6740(3) 0.62459(17) 0.40552(15) 0.0529(7) Uani 1 1 d . . . . .
O5 O 0.8552(3) 0.7389(2) 0.46754(19) 0.0754(9) Uani 1 1 d . . . . .
S1 S 0.75061(9) 0.71981(7) 0.40246(6) 0.0430(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.499(4) . ?
C1 C2 1.500(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.468(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.478(4) . ?
C3 C4 1.504(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.505(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.492(4) . ?
C5 C6 1.510(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N2 1.502(4) . ?
C7 C8 1.522(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N4 1.486(5) . ?
C9 C10 1.508(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 N4 1.504(4) . ?
C11 C12 1.521(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
N1 O2 1.202(4) . ?
N1 O1 1.214(4) . ?
N1 Pd1 2.022(3) . ?
N2 Pd1 2.086(2) . ?
N3 Pd1 2.004(2) . ?
N3 H3 0.9900 . ?
N4 Pd1 2.091(2) . ?
C13 F2 1.316(4) . ?
C13 F3 1.322(4) . ?
C13 F1 1.327(4) . ?
C13 S1 1.807(4) . ?
O3 S1 1.433(3) . ?
O4 S1 1.442(2) . ?
O5 S1 1.426(3) . ?

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
N2 C1 C2 110.3(3) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.9(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.9(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 111.0(3) . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
N4 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 113.7(3) . . ?
N2 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
N2 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 115.7(3) . . ?
N2 C7 H7A 108.4 . . ?
C8 C7 H7A 108.4 . . ?
N2 C7 H7B 108.4 . . ?
C8 C7 H7B 108.4 . . ?
H7A C7 H7B 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.7(3) . . ?
N4 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
N4 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 115.8(3) . . ?
N4 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N4 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 N1 O1 117.8(3) . . ?
O2 N1 Pd1 123.6(3) . . ?
O1 N1 Pd1 118.6(3) . . ?
C5 N2 C1 110.7(3) . . ?
C5 N2 C7 110.3(3) . . ?
C1 N2 C7 110.5(3) . . ?
C5 N2 Pd1 114.4(2) . . ?
C1 N2 Pd1 104.83(18) . . ?
C7 N2 Pd1 105.95(18) . . ?
C2 N3 C3 117.6(3) . . ?
C2 N3 Pd1 108.54(18) . . ?
C3 N3 Pd1 107.77(18) . . ?
C2 N3 H3 107.5 . . ?
C3 N3 H3 107.5 . . ?
Pd1 N3 H3 107.5 . . ?
C9 N4 C11 110.9(3) . . ?
C9 N4 C4 110.1(3) . . ?
C11 N4 C4 110.0(3) . . ?
C9 N4 Pd1 114.7(2) . . ?
C11 N4 Pd1 105.49(19) . . ?
C4 N4 Pd1 105.35(18) . . ?
N3 Pd1 N1 179.02(12) . . ?
N3 Pd1 N2 84.87(10) . . ?
N1 Pd1 N2 94.77(11) . . ?
N3 Pd1 N4 84.96(10) . . ?
N1 Pd1 N4 95.29(11) . . ?
N2 Pd1 N4 167.95(10) . . ?
F2 C13 F3 106.6(3) . . ?
F2 C13 F1 107.1(3) . . ?
F3 C13 F1 107.3(3) . . ?
F2 C13 S1 112.1(3) . . ?
F3 C13 S1 111.1(3) . . ?
F1 C13 S1 112.3(2) . . ?
O5 S1 O3 116.26(19) . . ?
O5 S1 O4 114.94(18) . . ?
O3 S1 O4 113.91(16) . . ?
O5 S1 C13 103.08(18) . . ?
O3 S1 C13 103.27(17) . . ?
O4 S1 C13 102.87(16) . . ?

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
N2 C1 C2 N3 -55.9(3) . . . . ?
N3 C3 C4 N4 54.2(3) . . . . ?
C6 C5 N2 C1 -70.1(4) . . . . ?
C6 C5 N2 C7 167.3(3) . . . . ?
C6 C5 N2 Pd1 48.0(4) . . . . ?
C2 C1 N2 C5 161.0(3) . . . . ?
C2 C1 N2 C7 -76.6(3) . . . . ?
C2 C1 N2 Pd1 37.2(3) . . . . ?
C8 C7 N2 C5 58.1(4) . . . . ?
C8 C7 N2 C1 -64.6(4) . . . . ?
C8 C7 N2 Pd1 -177.6(3) . . . . ?
C1 C2 N3 C3 168.2(2) . . . . ?
C1 C2 N3 Pd1 45.7(3) . . . . ?
C4 C3 N3 C2 -171.0(3) . . . . ?
C4 C3 N3 Pd1 -48.0(3) . . . . ?
C10 C9 N4 C11 -166.0(3) . . . . ?
C10 C9 N4 C4 72.0(4) . . . . ?
C10 C9 N4 Pd1 -46.6(4) . . . . ?
C12 C11 N4 C9 -56.3(4) . . . . ?
C12 C11 N4 C4 65.8(4) . . . . ?
C12 C11 N4 Pd1 178.9(3) . . . . ?
C3 C4 N4 C9 -156.7(3) . . . . ?
C3 C4 N4 C11 80.8(3) . . . . ?
C3 C4 N4 Pd1 -32.5(3) . . . . ?
F2 C13 S1 O5 -59.8(3) . . . . ?
F3 C13 S1 O5 -179.0(3) . . . . ?
F1 C13 S1 O5 60.8(3) . . . . ?
F2 C13 S1 O3 178.7(3) . . . . ?
F3 C13 S1 O3 59.5(3) . . . . ?
F1 C13 S1 O3 -60.6(3) . . . . ?
F2 C13 S1 O4 60.0(3) . . . . ?
F3 C13 S1 O4 -59.2(3) . . . . ?
F1 C13 S1 O4 -179.4(3) . . . . ?

_refine_diff_density_max         0.496
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.082

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_Pt_VT_150K
_database_code_depnum_ccdc_archive 'CCDC 1564470'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_Pt_VT_150K          
;
PROBLEM: Check Calcd Residual Density  0.91A From     Pt1       1.62 eA-3
RESPONSE: The residual density around the heavy Pt1 atom may be the result of fourier transform termination ripples, resulting from slightly reduced diffraction quality following a long period of photo-irradiation with this crystal (< 3 hrs).
;
# Added during the CSD deposition process: Tuesday 25 July 2017 11:25 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3149(4)
_cell_length_b                   13.0139(5)
_cell_length_c                   16.7987(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.765(5)
_cell_angle_gamma                90
_cell_volume                     2012.61(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3072
_cell_measurement_theta_min      3.8070
_cell_measurement_theta_max      29.2690

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.134
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9337
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.363
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4105
_reflns_number_gt                3256
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0435P)²+0.5651P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4105
_refine_ls_number_parameters     249
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0826
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.047
_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 0.5133(7) 0.5620(5) 0.1858(4) 0.0355(13) Uani 1 1 d . U . . .
H1A H 0.6049 0.5523 0.1637 0.043 Uiso 1 1 calc R U . . .
H1B H 0.4617 0.6216 0.1582 0.043 Uiso 1 1 calc R U . . .
C2 C 0.5475(7) 0.5838(5) 0.2743(4) 0.0358(13) Uani 1 1 d . U . . .
H2A H 0.6107 0.5294 0.3019 0.043 Uiso 1 1 calc R U . . .
H2B H 0.5976 0.6507 0.2838 0.043 Uiso 1 1 calc R U . . .
C3 C 0.4112(7) 0.5844(5) 0.3927(4) 0.0387(14) Uani 1 1 d . U . . .
H3A H 0.4463 0.6512 0.4164 0.046 Uiso 1 1 calc R U . . .
H3B H 0.4772 0.5296 0.4173 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2580(8) 0.5643(5) 0.4076(4) 0.0367(13) Uani 1 1 d . U . . .
H4A H 0.2560 0.5586 0.4662 0.044 Uiso 1 1 calc R U . . .
H4B H 0.1943 0.6221 0.3864 0.044 Uiso 1 1 calc R U . . .
C5 C 0.3412(8) 0.4679(5) 0.0852(4) 0.0385(14) Uani 1 1 d . U . . .
H5A H 0.2962 0.3997 0.0728 0.046 Uiso 1 1 calc R U . . .
H5B H 0.4123 0.4793 0.0480 0.046 Uiso 1 1 calc R U . . .
C6 C 0.2235(9) 0.5498(5) 0.0697(5) 0.0486(19) Uani 1 1 d . U . . .
H6A H 0.1733 0.5437 0.0143 0.073 Uiso 1 1 calc R U . . .
H6B H 0.2679 0.6180 0.0776 0.073 Uiso 1 1 calc R U . . .
H6C H 0.1537 0.5403 0.1072 0.073 Uiso 1 1 calc R U . . .
C7 C 0.5164(7) 0.3726(5) 0.1815(4) 0.0382(14) Uani 1 1 d . U . . .
H7A H 0.5722 0.3759 0.2365 0.046 Uiso 1 1 calc R U . . .
H7B H 0.4530 0.3113 0.1792 0.046 Uiso 1 1 calc R U . . .
C8 C 0.6222(8) 0.3566(6) 0.1234(5) 0.0507(19) Uani 1 1 d . U . . .
H8A H 0.5690 0.3507 0.0686 0.076 Uiso 1 1 calc R U . . .
H8B H 0.6777 0.2935 0.1375 0.076 Uiso 1 1 calc R U . . .
H8C H 0.6889 0.4152 0.1263 0.076 Uiso 1 1 calc R U . . .
C9 C 0.0406(7) 0.4608(5) 0.3571(5) 0.0388(15) Uani 1 1 d . U . . .
H9A H 0.0103 0.4698 0.4107 0.047 Uiso 1 1 calc R U . . .
H9B H 0.0085 0.3917 0.3370 0.047 Uiso 1 1 calc R U . . .
C10 C -0.0342(9) 0.5409(6) 0.3003(6) 0.063(2) Uani 1 1 d . U . . .
H10A H 0.0028 0.5371 0.2488 0.095 Uiso 1 1 calc R U . . .
H10B H -0.0149 0.6093 0.3238 0.095 Uiso 1 1 calc R U . . .
H10C H -0.1391 0.5281 0.2913 0.095 Uiso 1 1 calc R U . . .
C11 C 0.2649(7) 0.3751(5) 0.4160(4) 0.0363(13) Uani 1 1 d . U . . .
H11A H 0.2378 0.3120 0.3843 0.044 Uiso 1 1 calc R U . . .
H11B H 0.3721 0.3802 0.4239 0.044 Uiso 1 1 calc R U . . .
C12 C 0.2183(8) 0.3622(6) 0.4971(5) 0.0472(18) Uani 1 1 d . U . . .
H12A H 0.1130 0.3511 0.4904 0.071 Uiso 1 1 calc R U . . .
H12B H 0.2432 0.4241 0.5295 0.071 Uiso 1 1 calc R U . . .
H12C H 0.2681 0.3027 0.5245 0.071 Uiso 1 1 calc R U . . .
N2 N 0.4198(6) 0.4668(4) 0.1693(3) 0.0319(9) Uani 1 1 d . U . . .
N3 N 0.4066(5) 0.5858(4) 0.3040(3) 0.0322(11) Uani 1 1 d . U . . .
H3 H 0.3528 0.6488 0.2822 0.039 Uiso 1 1 calc R U . . .
N4 N 0.2037(6) 0.4662(4) 0.3663(3) 0.0283(9) Uani 1 1 d . U . . .
Pt1 Pt 0.29212(2) 0.46209(2) 0.26031(2) 0.02665(10) Uani 1 1 d . U . . .
N1 N 0.1875(3) 0.3296(4) 0.22087(16) 0.0405(10) Uani 0.333(8) 1 d D U P A 1
O1 O 0.2342(8) 0.2495(8) 0.2417(4) 0.075(2) Uani 0.333(8) 1 d D U P A 1
O2 O 0.0758(8) 0.3431(11) 0.1752(4) 0.075(2) Uani 0.333(8) 1 d D U P A 1
N1A N 0.0655(6) 0.3194(6) 0.1715(3) 0.0405(10) Uani 0.667(8) 1 d D U P A 2
O1A O 0.1875(3) 0.3296(4) 0.22087(16) 0.0405(10) Uani 0.667(8) 1 d D U P A 2
O2A O 0.0145(7) 0.4077(5) 0.1488(4) 0.075(2) Uani 0.667(8) 1 d D U P A 2
C13 C 0.6085(7) 0.1975(5) 0.4038(4) 0.0336(9) Uani 1 1 d . U . . .
F1 F 0.6543(4) 0.1010(3) 0.4004(2) 0.0439(9) Uani 1 1 d . U . . .
F2 F 0.4956(4) 0.2097(3) 0.3456(3) 0.0439(9) Uani 1 1 d . U . . .
F3 F 0.5600(4) 0.2087(3) 0.4741(3) 0.0492(10) Uani 1 1 d . U . . .
O3 O 0.7900(5) 0.2638(3) 0.3161(3) 0.0441(11) Uani 1 1 d . U . . .
O4 O 0.6811(5) 0.3861(3) 0.3974(3) 0.0429(11) Uani 1 1 d . U . . .
O5 O 0.8599(5) 0.2646(4) 0.4616(3) 0.0492(12) Uani 1 1 d . U . . .
S1 S 0.75258(17) 0.28800(12) 0.39366(11) 0.0336(4) Uani 1 1 d . 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
C1 C2 1.498(9) . ?
C1 N2 1.516(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.473(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.484(8) . ?
C3 C4 1.509(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.503(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.488(9) . ?
C5 C6 1.522(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.503(9) . ?
C7 N2 1.515(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.505(8) . ?
C9 C10 1.510(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.502(9) . ?
C11 N4 1.510(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.076(5) . ?
N3 Pt1 2.008(5) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.074(5) . ?
Pt1 O1A 2.041(4) . ?
Pt1 N1 2.041(4) . ?
N1 O1 1.163(8) . ?
N1 O2 1.209(8) . ?
N1A O2A 1.280(8) . ?
N1A O1A 1.307(7) . ?
C13 F1 1.331(7) . ?
C13 F2 1.332(7) . ?
C13 F3 1.336(8) . ?
C13 S1 1.813(6) . ?
O3 S1 1.434(5) . ?
O4 S1 1.446(5) . ?
O5 S1 1.431(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 111.5(5) . . ?
C2 C1 H1A 109.3 . . ?
N2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
N2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 105.9(5) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.5(6) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 109.4(5) . . ?
N4 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N4 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.0(6) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N2 117.3(6) . . ?
C8 C7 H7A 108.0 . . ?
N2 C7 H7A 108.0 . . ?
C8 C7 H7B 108.0 . . ?
N2 C7 H7B 108.0 . . ?
H7A C7 H7B 107.2 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.2(6) . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 116.9(5) . . ?
C12 C11 H11A 108.1 . . ?
N4 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
N4 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C7 109.5(5) . . ?
C5 N2 C1 110.6(5) . . ?
C7 N2 C1 108.9(5) . . ?
C5 N2 Pt1 116.4(4) . . ?
C7 N2 Pt1 105.8(4) . . ?
C1 N2 Pt1 105.4(4) . . ?
C2 N3 C3 116.7(5) . . ?
C2 N3 Pt1 108.2(4) . . ?
C3 N3 Pt1 106.8(4) . . ?
C2 N3 H3 108.3 . . ?
C3 N3 H3 108.3 . . ?
Pt1 N3 H3 108.3 . . ?
C4 N4 C9 110.5(5) . . ?
C4 N4 C11 109.9(5) . . ?
C9 N4 C11 108.0(5) . . ?
C4 N4 Pt1 105.5(4) . . ?
C9 N4 Pt1 116.0(4) . . ?
C11 N4 Pt1 106.7(4) . . ?
N3 Pt1 O1A 175.64(19) . . ?
N3 Pt1 N1 175.64(19) . . ?
N3 Pt1 N4 85.6(2) . . ?
O1A Pt1 N4 93.90(15) . . ?
N1 Pt1 N4 93.90(15) . . ?
N3 Pt1 N2 85.1(2) . . ?
O1A Pt1 N2 94.84(16) . . ?
N1 Pt1 N2 94.84(16) . . ?
N4 Pt1 N2 168.2(2) . . ?
O1 N1 O2 124.6(9) . . ?
O1 N1 Pt1 121.5(5) . . ?
O2 N1 Pt1 113.9(8) . . ?
O2A N1A O1A 110.2(6) . . ?
N1A O1A Pt1 128.1(4) . . ?
F1 C13 F2 107.6(5) . . ?
F1 C13 F3 107.2(5) . . ?
F2 C13 F3 107.5(5) . . ?
F1 C13 S1 111.2(4) . . ?
F2 C13 S1 111.5(4) . . ?
F3 C13 S1 111.6(4) . . ?
O5 S1 O3 116.2(3) . . ?
O5 S1 O4 115.0(3) . . ?
O3 S1 O4 114.3(3) . . ?
O5 S1 C13 103.0(3) . . ?
O3 S1 C13 103.2(3) . . ?
O4 S1 C13 102.6(3) . . ?

_refine_diff_density_max         1.898
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.172

####################################################################### 
# 
# 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_GS_100K
_database_code_depnum_ccdc_archive 'CCDC 1564449'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)palladium(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pd, C F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pd S'
_chemical_formula_weight         516.86

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2030(3)
_cell_length_b                   13.1728(5)
_cell_length_c                   16.9033(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.338(4)
_cell_angle_gamma                90
_cell_volume                     2032.39(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3910
_cell_measurement_theta_min      3.9450
_cell_measurement_theta_max      29.5540

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.074
_shelx_estimated_absorpt_T_min   0.644
_shelx_estimated_absorpt_T_max   0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9352
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.323
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4145
_reflns_number_gt                3456
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0164P)²+0.2757P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4145
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0603
_refine_ls_wR_factor_gt          0.0558
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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 0.2567(3) 0.43814(19) 0.40866(16) 0.0191(6) Uani 1 1 d . . . . .
H1A H 0.1930 0.3830 0.3843 0.023 Uiso 1 1 calc R U . . .
H1B H 0.2476 0.4404 0.4664 0.023 Uiso 1 1 calc R U . . .
C2 C 0.4139(3) 0.4169(2) 0.39708(15) 0.0170(6) Uani 1 1 d . . . . .
H2A H 0.4800 0.4687 0.4247 0.020 Uiso 1 1 calc R U . . .
H2B H 0.4445 0.3491 0.4184 0.020 Uiso 1 1 calc R U . . .
C3 C 0.5634(3) 0.4229(2) 0.28132(16) 0.0170(6) Uani 1 1 d . . . . .
H3A H 0.6138 0.3569 0.2915 0.020 Uiso 1 1 calc R U . . .
H3B H 0.6255 0.4769 0.3087 0.020 Uiso 1 1 calc R U . . .
C4 C 0.5346(3) 0.44368(19) 0.19303(16) 0.0184(6) Uani 1 1 d . . . . .
H4A H 0.6288 0.4520 0.1714 0.022 Uiso 1 1 calc R U . . .
H4B H 0.4822 0.3853 0.1657 0.022 Uiso 1 1 calc R U . . .
C5 C 0.0456(3) 0.5446(2) 0.35818(16) 0.0218(6) Uani 1 1 d . . . . .
H5A H 0.0173 0.6156 0.3444 0.026 Uiso 1 1 calc R U . . .
H5B H 0.0073 0.5277 0.4087 0.026 Uiso 1 1 calc R U . . .
C6 C -0.0253(3) 0.4750(2) 0.29293(18) 0.0308(7) Uani 1 1 d . . . . .
H6A H 0.0136 0.4903 0.2429 0.046 Uiso 1 1 calc R U . . .
H6B H -0.1316 0.4856 0.2858 0.046 Uiso 1 1 calc R U . . .
H6C H -0.0037 0.4042 0.3079 0.046 Uiso 1 1 calc R U . . .
C7 C 0.2718(3) 0.62480(19) 0.42159(15) 0.0184(6) Uani 1 1 d . . . . .
H7A H 0.2491 0.6886 0.3916 0.022 Uiso 1 1 calc R U . . .
H7B H 0.3798 0.6175 0.4301 0.022 Uiso 1 1 calc R U . . .
C8 C 0.2173(3) 0.6348(2) 0.50290(16) 0.0264(7) Uani 1 1 d . . . . .
H8A H 0.1126 0.6513 0.4954 0.040 Uiso 1 1 calc R U . . .
H8B H 0.2716 0.6890 0.5335 0.040 Uiso 1 1 calc R U . . .
H8C H 0.2327 0.5705 0.5320 0.040 Uiso 1 1 calc R U . . .
C9 C 0.3653(3) 0.5363(2) 0.09430(15) 0.0199(6) Uani 1 1 d . . . . .
H9A H 0.4357 0.5177 0.0570 0.024 Uiso 1 1 calc R U . . .
H9B H 0.3282 0.6053 0.0799 0.024 Uiso 1 1 calc R U . . .
C10 C 0.2385(3) 0.4626(2) 0.08368(16) 0.0242(6) Uani 1 1 d . . . . .
H10A H 0.1943 0.4626 0.0278 0.036 Uiso 1 1 calc R U . . .
H10B H 0.1651 0.4831 0.1177 0.036 Uiso 1 1 calc R U . . .
H10C H 0.2740 0.3942 0.0987 0.036 Uiso 1 1 calc R U . . .
C11 C 0.5397(3) 0.63123(19) 0.18984(16) 0.0199(6) Uani 1 1 d . . . . .
H11A H 0.5939 0.6280 0.2443 0.024 Uiso 1 1 calc R U . . .
H11B H 0.4758 0.6919 0.1874 0.024 Uiso 1 1 calc R U . . .
C12 C 0.6504(3) 0.6456(2) 0.13067(18) 0.0315(7) Uani 1 1 d . . . . .
H12A H 0.5982 0.6587 0.0774 0.047 Uiso 1 1 calc R U . . .
H12B H 0.7098 0.5840 0.1293 0.047 Uiso 1 1 calc R U . . .
H12C H 0.7143 0.7033 0.1473 0.047 Uiso 1 1 calc R U . . .
N1 N 0.1974(2) 0.66928(16) 0.22354(13) 0.0176(5) Uani 1 1 d . . . . .
N2 N 0.2086(2) 0.53737(15) 0.37087(12) 0.0146(5) Uani 1 1 d . . . . .
N3 N 0.4181(2) 0.42095(15) 0.31006(12) 0.0120(4) Uani 1 1 d . . . . .
H3 H 0.3647 0.3600 0.2861 0.014 Uiso 1 1 calc R U . . .
N4 N 0.4438(2) 0.53840(15) 0.17710(12) 0.0147(5) Uani 1 1 d . . . . .
O1 O 0.2397(3) 0.75169(15) 0.25382(13) 0.0384(6) Uani 1 1 d . . . . .
O2 O 0.0928(3) 0.66799(15) 0.17192(13) 0.0400(6) Uani 1 1 d . . . . .
Pd1 Pd 0.30734(2) 0.54373(2) 0.26654(2) 0.01126(7) Uani 1 1 d . . . . .
C13 C 0.6101(3) 0.81105(19) 0.41127(16) 0.0190(6) Uani 1 1 d . . . . .
F1 F 0.66148(18) 0.90628(11) 0.40916(10) 0.0262(4) Uani 1 1 d . . . . .
F2 F 0.55676(18) 0.80048(12) 0.48035(9) 0.0294(4) Uani 1 1 d . . . . .
F3 F 0.49962(18) 0.80291(12) 0.35297(10) 0.0299(4) Uani 1 1 d . . . . .
O3 O 0.7960(2) 0.74282(14) 0.32356(12) 0.0255(5) Uani 1 1 d . . . . .
O4 O 0.6751(2) 0.62293(13) 0.40215(11) 0.0215(4) Uani 1 1 d . . . . .
O5 O 0.8596(2) 0.73718(15) 0.46813(12) 0.0289(5) Uani 1 1 d . . . . .
S1 S 0.75247(7) 0.71831(5) 0.40009(4) 0.01737(15) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.497(3) . ?
C1 C2 1.511(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.477(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.480(3) . ?
C3 C4 1.507(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.507(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.491(3) . ?
C5 C6 1.516(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.508(3) . ?
C7 C8 1.528(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.491(3) . ?
C9 C10 1.511(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.507(3) . ?
C11 C12 1.528(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 O2 1.214(3) . ?
N1 O1 1.242(3) . ?
N1 Pd1 2.025(2) . ?
N2 Pd1 2.086(2) . ?
N3 Pd1 2.001(2) . ?
N3 H3 1.0000 . ?
N4 Pd1 2.086(2) . ?
C13 F3 1.327(3) . ?
C13 F2 1.331(3) . ?
C13 F1 1.343(3) . ?
C13 S1 1.819(3) . ?
O3 S1 1.4391(19) . ?
O4 S1 1.4468(18) . ?
O5 S1 1.438(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
N2 C1 C2 110.0(2) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 105.6(2) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.0(2) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.5(2) . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 113.4(2) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 115.5(2) . . ?
N2 C7 H7A 108.4 . . ?
C8 C7 H7A 108.4 . . ?
N2 C7 H7B 108.4 . . ?
C8 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.4(2) . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 115.7(2) . . ?
N4 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N4 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 N1 O1 119.1(2) . . ?
O2 N1 Pd1 124.10(17) . . ?
O1 N1 Pd1 116.74(18) . . ?
C5 N2 C1 110.8(2) . . ?
C5 N2 C7 109.93(19) . . ?
C1 N2 C7 110.7(2) . . ?
C5 N2 Pd1 114.50(16) . . ?
C1 N2 Pd1 105.00(14) . . ?
C7 N2 Pd1 105.78(15) . . ?
C2 N3 C3 117.9(2) . . ?
C2 N3 Pd1 108.55(15) . . ?
C3 N3 Pd1 107.73(15) . . ?
C2 N3 H3 107.4 . . ?
C3 N3 H3 107.4 . . ?
Pd1 N3 H3 107.4 . . ?
C9 N4 C4 110.09(19) . . ?
C9 N4 C11 110.73(19) . . ?
C4 N4 C11 110.2(2) . . ?
C9 N4 Pd1 114.61(16) . . ?
C4 N4 Pd1 105.65(14) . . ?
C11 N4 Pd1 105.36(15) . . ?
N3 Pd1 N1 179.15(9) . . ?
N3 Pd1 N2 85.02(8) . . ?
N1 Pd1 N2 94.85(8) . . ?
N3 Pd1 N4 85.05(8) . . ?
N1 Pd1 N4 94.98(8) . . ?
N2 Pd1 N4 168.16(8) . . ?
F3 C13 F2 108.0(2) . . ?
F3 C13 F1 107.1(2) . . ?
F2 C13 F1 107.0(2) . . ?
F3 C13 S1 111.25(18) . . ?
F2 C13 S1 111.86(18) . . ?
F1 C13 S1 111.36(18) . . ?
O5 S1 O3 116.04(13) . . ?
O5 S1 O4 114.85(12) . . ?
O3 S1 O4 114.27(11) . . ?
O5 S1 C13 103.32(12) . . ?
O3 S1 C13 103.28(12) . . ?
O4 S1 C13 102.56(12) . . ?

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
N2 C1 C2 N3 -56.1(3) . . . . ?
N3 C3 C4 N4 54.1(3) . . . . ?
C6 C5 N2 C1 -70.8(3) . . . . ?
C6 C5 N2 C7 166.6(2) . . . . ?
C6 C5 N2 Pd1 47.7(3) . . . . ?
C2 C1 N2 C5 161.8(2) . . . . ?
C2 C1 N2 C7 -76.0(3) . . . . ?
C2 C1 N2 Pd1 37.7(2) . . . . ?
C8 C7 N2 C5 57.0(3) . . . . ?
C8 C7 N2 C1 -65.7(3) . . . . ?
C8 C7 N2 Pd1 -178.93(19) . . . . ?
C1 C2 N3 C3 168.3(2) . . . . ?
C1 C2 N3 Pd1 45.6(2) . . . . ?
C4 C3 N3 C2 -171.2(2) . . . . ?
C4 C3 N3 Pd1 -48.1(2) . . . . ?
C10 C9 N4 C4 73.4(3) . . . . ?
C10 C9 N4 C11 -164.5(2) . . . . ?
C10 C9 N4 Pd1 -45.5(3) . . . . ?
C3 C4 N4 C9 -156.8(2) . . . . ?
C3 C4 N4 C11 80.8(3) . . . . ?
C3 C4 N4 Pd1 -32.6(2) . . . . ?
C12 C11 N4 C9 -55.1(3) . . . . ?
C12 C11 N4 C4 66.9(3) . . . . ?
C12 C11 N4 Pd1 -179.5(2) . . . . ?
F3 C13 S1 O5 -179.01(17) . . . . ?
F2 C13 S1 O5 -58.1(2) . . . . ?
F1 C13 S1 O5 61.5(2) . . . . ?
F3 C13 S1 O3 59.7(2) . . . . ?
F2 C13 S1 O3 -179.38(18) . . . . ?
F1 C13 S1 O3 -59.8(2) . . . . ?
F3 C13 S1 O4 -59.3(2) . . . . ?
F2 C13 S1 O4 61.6(2) . . . . ?
F1 C13 S1 O4 -178.78(18) . . . . ?

_refine_diff_density_max         0.484
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.089

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_Pt_MS2h_100K
_database_code_depnum_ccdc_archive 'CCDC 1564463'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2881(4)
_cell_length_b                   13.0071(5)
_cell_length_c                   16.7446(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.816(4)
_cell_angle_gamma                90
_cell_volume                     1999.04(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3905
_cell_measurement_theta_min      4.0300
_cell_measurement_theta_max      28.7900

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.182
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.162
_exptl_absorpt_correction_T_max  0.643
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9910
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.366
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4079
_reflns_number_gt                3312
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0289P)²+0.4992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4079
_refine_ls_number_parameters     257
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.036
_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 0.5139(7) 0.5627(4) 0.1858(4) 0.0316(12) Uani 1 1 d . U . . .
H1A H 0.6055 0.5538 0.1632 0.038 Uiso 1 1 calc R U . . .
H1B H 0.4612 0.6224 0.1587 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5486(6) 0.5828(5) 0.2751(4) 0.0324(12) Uani 1 1 d . U . . .
H2A H 0.6113 0.5276 0.3022 0.039 Uiso 1 1 calc R U . . .
H2B H 0.5998 0.6494 0.2855 0.039 Uiso 1 1 calc R U . . .
C3 C 0.4128(7) 0.5854(5) 0.3942(3) 0.0329(12) Uani 1 1 d . U . . .
H3A H 0.4465 0.6530 0.4172 0.040 Uiso 1 1 calc R U . . .
H3B H 0.4800 0.5315 0.4196 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2595(6) 0.5641(4) 0.4084(4) 0.0292(11) Uani 1 1 d . U . . .
H4A H 0.1954 0.6219 0.3871 0.035 Uiso 1 1 calc R U . . .
H4B H 0.2572 0.5585 0.4671 0.035 Uiso 1 1 calc R U . . .
C5 C 0.3410(6) 0.4675(4) 0.0849(3) 0.0295(11) Uani 1 1 d . U . . .
H5A H 0.2958 0.3993 0.0727 0.035 Uiso 1 1 calc R U . . .
H5B H 0.4118 0.4789 0.0472 0.035 Uiso 1 1 calc R U . . .
C6 C 0.2237(7) 0.5492(4) 0.0702(4) 0.0365(14) Uani 1 1 d . U . . .
H6A H 0.1725 0.5434 0.0147 0.055 Uiso 1 1 calc R U . . .
H6B H 0.2684 0.6174 0.0783 0.055 Uiso 1 1 calc R U . . .
H6C H 0.1543 0.5395 0.1082 0.055 Uiso 1 1 calc R U . . .
C7 C 0.5179(6) 0.3722(4) 0.1815(4) 0.0315(12) Uani 1 1 d . U . . .
H7A H 0.5745 0.3752 0.2366 0.038 Uiso 1 1 calc R U . . .
H7B H 0.4546 0.3107 0.1791 0.038 Uiso 1 1 calc R U . . .
C8 C 0.6228(7) 0.3574(5) 0.1227(4) 0.0427(16) Uani 1 1 d . U . . .
H8A H 0.5685 0.3466 0.0684 0.064 Uiso 1 1 calc R U . . .
H8B H 0.6842 0.2973 0.1387 0.064 Uiso 1 1 calc R U . . .
H8C H 0.6843 0.4186 0.1227 0.064 Uiso 1 1 calc R U . . .
C9 C 0.0413(6) 0.4615(4) 0.3576(4) 0.0310(12) Uani 1 1 d . U . . .
H9A H 0.0109 0.4718 0.4112 0.037 Uiso 1 1 calc R U . . .
H9B H 0.0088 0.3921 0.3384 0.037 Uiso 1 1 calc R U . . .
C10 C -0.0345(8) 0.5402(5) 0.2997(5) 0.0527(19) Uani 1 1 d . U . . .
H10A H -0.0064 0.5300 0.2461 0.079 Uiso 1 1 calc R U . . .
H10B H -0.0060 0.6094 0.3192 0.079 Uiso 1 1 calc R U . . .
H10C H -0.1402 0.5323 0.2960 0.079 Uiso 1 1 calc R U . . .
C11 C 0.2659(6) 0.3738(4) 0.4165(3) 0.0304(12) Uani 1 1 d . U . . .
H11A H 0.2379 0.3110 0.3844 0.036 Uiso 1 1 calc R U . . .
H11B H 0.3735 0.3785 0.4242 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2197(7) 0.3605(5) 0.4983(4) 0.0371(14) Uani 1 1 d . U . . .
H12A H 0.1164 0.3417 0.4915 0.056 Uiso 1 1 calc R U . . .
H12B H 0.2346 0.4252 0.5285 0.056 Uiso 1 1 calc R U . . .
H12C H 0.2780 0.3061 0.5281 0.056 Uiso 1 1 calc R U . . .
N2 N 0.4208(5) 0.4668(3) 0.1694(3) 0.0263(8) Uani 1 1 d . U . . .
N3 N 0.4074(5) 0.5852(3) 0.3054(3) 0.0279(9) Uani 1 1 d . U . . .
H3 H 0.3536 0.6481 0.2832 0.033 Uiso 1 1 calc R U . . .
N4 N 0.2043(5) 0.4658(3) 0.3672(3) 0.0247(8) Uani 1 1 d . U . . .
Pt1 Pt 0.29304(2) 0.46215(2) 0.26066(2) 0.02278(8) Uani 1 1 d . U . . .
N1 N 0.1863(3) 0.3309(3) 0.22004(13) 0.0328(9) Uani 0.400(7) 1 d D U P A 1
O1 O 0.2373(7) 0.2530(6) 0.2439(3) 0.063(2) Uani 0.400(7) 1 d D U P A 1
O2 O 0.0750(7) 0.3417(9) 0.1730(3) 0.063(2) Uani 0.400(7) 1 d D U P A 1
N1A N 0.0652(7) 0.3203(7) 0.1696(3) 0.0328(9) Uani 0.501(8) 1 d D U P A 2
O1A O 0.1863(3) 0.3309(3) 0.22004(13) 0.0328(9) Uani 0.501(8) 1 d D U P A 2
O2A O 0.0170(8) 0.4087(6) 0.1466(4) 0.063(2) Uani 0.501(8) 1 d D U P A 2
O1B O 0.1863(3) 0.3309(3) 0.22004(13) 0.0328(9) Uani 0.099(8) 1 d D U P A 3
N1B N 0.0756(11) 0.3707(18) 0.1723(5) 0.0328(9) Uani 0.099(8) 1 d D U P A 3
O2B O -0.0062(11) 0.296(3) 0.1404(5) 0.063(2) Uani 0.099(8) 1 d D U P A 3
C13 C 0.6087(6) 0.1973(4) 0.4040(3) 0.0249(8) Uani 1 1 d . U . . .
F1 F 0.6543(4) 0.1002(2) 0.4006(2) 0.0345(8) Uani 1 1 d . U . . .
F2 F 0.4948(3) 0.2090(2) 0.3451(2) 0.0335(8) Uani 1 1 d . U . . .
F3 F 0.5601(4) 0.2079(2) 0.4744(2) 0.0377(8) Uani 1 1 d . U . . .
O3 O 0.7895(5) 0.2627(3) 0.3154(2) 0.0357(9) Uani 1 1 d . U . . .
O4 O 0.6810(4) 0.3863(3) 0.3970(2) 0.0339(9) Uani 1 1 d . U . . .
O5 O 0.8609(4) 0.2646(3) 0.4618(3) 0.0379(10) Uani 1 1 d . U . . .
S1 S 0.75290(15) 0.28765(10) 0.39349(9) 0.0273(3) Uani 1 1 d . 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
C1 C2 1.505(8) . ?
C1 N2 1.519(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.477(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.481(7) . ?
C3 C4 1.505(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.505(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.493(7) . ?
C5 C6 1.514(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.499(8) . ?
C7 N2 1.520(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.499(7) . ?
C9 C10 1.508(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.506(8) . ?
C11 N4 1.516(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.074(5) . ?
N3 Pt1 2.002(4) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.076(5) . ?
Pt1 O1B 2.038(4) . ?
Pt1 O1A 2.038(4) . ?
Pt1 N1 2.038(4) . ?
N1 O1 1.162(7) . ?
N1 O2 1.208(7) . ?
N1A O2A 1.272(8) . ?
N1A O1A 1.307(7) . ?
O1B N1B 1.308(10) . ?
N1B O2B 1.299(10) . ?
C13 F3 1.332(6) . ?
C13 F1 1.336(6) . ?
C13 F2 1.340(6) . ?
C13 S1 1.811(5) . ?
O3 S1 1.438(4) . ?
O4 S1 1.452(4) . ?
O5 S1 1.432(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 110.6(5) . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.2(5) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.7(5) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 110.4(5) . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
N4 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 113.5(5) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N2 116.7(5) . . ?
C8 C7 H7A 108.1 . . ?
N2 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
N2 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 114.0(5) . . ?
N4 C9 H9A 108.7 . . ?
C10 C9 H9A 108.7 . . ?
N4 C9 H9B 108.7 . . ?
C10 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 116.7(5) . . ?
C12 C11 H11A 108.1 . . ?
N4 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
N4 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 110.6(4) . . ?
C5 N2 C7 109.2(4) . . ?
C1 N2 C7 109.3(5) . . ?
C5 N2 Pt1 116.2(4) . . ?
C1 N2 Pt1 105.4(3) . . ?
C7 N2 Pt1 105.9(3) . . ?
C2 N3 C3 116.7(5) . . ?
C2 N3 Pt1 107.6(3) . . ?
C3 N3 Pt1 108.2(3) . . ?
C2 N3 H3 108.0 . . ?
C3 N3 H3 108.0 . . ?
Pt1 N3 H3 108.0 . . ?
C9 N4 C4 110.4(4) . . ?
C9 N4 C11 108.6(4) . . ?
C4 N4 C11 110.3(4) . . ?
C9 N4 Pt1 115.8(3) . . ?
C4 N4 Pt1 105.2(3) . . ?
C11 N4 Pt1 106.5(3) . . ?
N3 Pt1 O1B 176.16(16) . . ?
N3 Pt1 O1A 176.16(16) . . ?
N3 Pt1 N1 176.16(16) . . ?
N3 Pt1 N2 85.52(18) . . ?
O1B Pt1 N2 94.72(14) . . ?
O1A Pt1 N2 94.72(14) . . ?
N1 Pt1 N2 94.72(14) . . ?
N3 Pt1 N4 85.29(17) . . ?
O1B Pt1 N4 93.97(13) . . ?
O1A Pt1 N4 93.97(13) . . ?
N1 Pt1 N4 93.97(13) . . ?
N2 Pt1 N4 168.27(17) . . ?
O1 N1 O2 126.0(8) . . ?
O1 N1 Pt1 117.6(4) . . ?
O2 N1 Pt1 116.3(6) . . ?
O2A N1A O1A 109.3(7) . . ?
N1A O1A Pt1 129.0(4) . . ?
N1B O1B Pt1 99.7(11) . . ?
O2B N1B O1B 108.1(11) . . ?
F3 C13 F1 106.8(4) . . ?
F3 C13 F2 107.7(4) . . ?
F1 C13 F2 107.2(4) . . ?
F3 C13 S1 112.0(4) . . ?
F1 C13 S1 111.4(4) . . ?
F2 C13 S1 111.5(4) . . ?
O5 S1 O3 116.4(3) . . ?
O5 S1 O4 115.0(3) . . ?
O3 S1 O4 114.3(2) . . ?
O5 S1 C13 103.0(2) . . ?
O3 S1 C13 102.9(3) . . ?
O4 S1 C13 102.6(3) . . ?

_refine_diff_density_max         1.554
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.153

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
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data_Pt_MS2h_200K
_database_code_depnum_ccdc_archive 'CCDC 1564465'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3266(2)
_cell_length_b                   12.9762(3)
_cell_length_c                   16.7496(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.174(2)
_cell_angle_gamma                90
_cell_volume                     2001.17(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    10232
_cell_measurement_theta_min      3.9860
_cell_measurement_theta_max      29.5880

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 5 0.1067
-5 0 4 0.0512
1 5 -1 0.2318
-1 1 -5 0.1103
-1 -5 -3 0.2517
-1 0 -5 0.1033
5 0 -4 0.0348
0 -1 1 0.1437
-5 1 4 0.0508
-3 -5 2 0.1832
-3 5 2 0.1520
0 3 -5 0.1696
_exptl_absorpt_coefficient_mu    7.175
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            21889
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.373
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4087
_reflns_number_gt                3658
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0166P)²+1.1535P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4087
_refine_ls_number_parameters     255
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0181
_refine_ls_wR_factor_ref         0.0409
_refine_ls_wR_factor_gt          0.0394
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.004
_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 -0.0069(3) 0.5639(2) 0.81722(19) 0.0300(6) Uani 1 1 d . U . . .
H1A H -0.0978 0.5548 0.8399 0.036 Uiso 1 1 calc R U . . .
H1B H 0.0463 0.6234 0.8446 0.036 Uiso 1 1 calc R U . . .
C2 C -0.0428(3) 0.5848(2) 0.72780(19) 0.0290(6) Uani 1 1 d . U . . .
H2A H -0.1055 0.5296 0.7004 0.035 Uiso 1 1 calc R U . . .
H2B H -0.0940 0.6515 0.7178 0.035 Uiso 1 1 calc R U . . .
C3 C 0.0901(3) 0.5851(2) 0.60802(18) 0.0303(6) Uani 1 1 d . U . . .
H3A H 0.0541 0.6518 0.5839 0.036 Uiso 1 1 calc R U . . .
H3B H 0.0236 0.5298 0.5843 0.036 Uiso 1 1 calc R U . . .
C4 C 0.2422(4) 0.5647(2) 0.59255(19) 0.0304(6) Uani 1 1 d . U . . .
H4A H 0.3061 0.6231 0.6129 0.036 Uiso 1 1 calc R U . . .
H4B H 0.2425 0.5581 0.5337 0.036 Uiso 1 1 calc R U . . .
C5 C -0.0095(3) 0.3733(2) 0.81940(19) 0.0294(6) Uani 1 1 d . U . . .
H5A H 0.0546 0.3121 0.8223 0.035 Uiso 1 1 calc R U . . .
H5B H -0.0650 0.3762 0.7639 0.035 Uiso 1 1 calc R U . . .
C6 C -0.1168(4) 0.3568(3) 0.8778(2) 0.0417(8) Uani 1 1 d . U . . .
H6A H -0.1754 0.2953 0.8618 0.062 Uiso 1 1 calc R U . . .
H6B H -0.1806 0.4170 0.8766 0.062 Uiso 1 1 calc R U . . .
H6C H -0.0636 0.3475 0.9327 0.062 Uiso 1 1 calc R U . . .
C7 C 0.1661(4) 0.4680(2) 0.91762(18) 0.0294(6) Uani 1 1 d . U . . .
H7A H 0.2143 0.4003 0.9286 0.035 Uiso 1 1 calc R U . . .
H7B H 0.0953 0.4760 0.9554 0.035 Uiso 1 1 calc R U . . .
C8 C 0.2794(4) 0.5520(2) 0.9345(2) 0.0377(8) Uani 1 1 d . U . . .
H8A H 0.3429 0.5502 0.8932 0.057 Uiso 1 1 calc R U . . .
H8B H 0.3374 0.5411 0.9879 0.057 Uiso 1 1 calc R U . . .
H8C H 0.2312 0.6193 0.9332 0.057 Uiso 1 1 calc R U . . .
C9 C 0.2367(3) 0.3742(2) 0.58708(18) 0.0287(6) Uani 1 1 d . U . . .
H9A H 0.1295 0.3786 0.5801 0.034 Uiso 1 1 calc R U . . .
H9B H 0.2660 0.3118 0.6197 0.034 Uiso 1 1 calc R U . . .
C10 C 0.2804(4) 0.3596(3) 0.50396(19) 0.0373(8) Uani 1 1 d . U . . .
H10A H 0.2555 0.4216 0.4713 0.056 Uiso 1 1 calc R U . . .
H10B H 0.2286 0.3002 0.4771 0.056 Uiso 1 1 calc R U . . .
H10C H 0.3853 0.3475 0.5100 0.056 Uiso 1 1 calc R U . . .
C11 C 0.4616(3) 0.4631(2) 0.6439(2) 0.0331(7) Uani 1 1 d . U . . .
H11A H 0.4904 0.4688 0.5897 0.040 Uiso 1 1 calc R U . . .
H11B H 0.4954 0.3953 0.6667 0.040 Uiso 1 1 calc R U . . .
C12 C 0.5370(4) 0.5469(3) 0.6973(2) 0.0492(10) Uani 1 1 d . U . . .
H12A H 0.5262 0.6128 0.6683 0.074 Uiso 1 1 calc R U . . .
H12B H 0.6404 0.5302 0.7117 0.074 Uiso 1 1 calc R U . . .
H12C H 0.4933 0.5522 0.7467 0.074 Uiso 1 1 calc R U . . .
N2 N 0.0851(3) 0.46798(17) 0.83247(15) 0.0237(5) Uani 1 1 d . U . . .
N3 N 0.0985(2) 0.58772(18) 0.69761(14) 0.0231(5) Uani 1 1 d . U . . .
H3 H 0.1524 0.6511 0.7190 0.028 Uiso 1 1 calc R U . . .
N4 N 0.2985(3) 0.46680(17) 0.63482(15) 0.0233(5) Uani 1 1 d . U . . .
Pt1 Pt 0.21278(2) 0.46377(2) 0.74167(2) 0.01896(4) Uani 1 1 d . U . . .
N1 N 0.3129(2) 0.32794(15) 0.77950(13) 0.0293(5) Uani 0.079(4) 1 d D U P A 1
O1 O 0.272(2) 0.2476(11) 0.7520(13) 0.0293(5) Uani 0.079(4) 1 d D U P A 1
O2 O 0.418(3) 0.338(2) 0.8313(19) 0.0293(5) Uani 0.079(4) 1 d D U P A 1
N1A N 0.4392(4) 0.3229(3) 0.8283(3) 0.0408(9) Uani 0.921(4) 1 d D U P A 2
O1A O 0.3129(2) 0.32794(15) 0.77950(13) 0.0293(5) Uani 0.921(4) 1 d D U P A 2
O2A O 0.4902(3) 0.4059(2) 0.84947(18) 0.0540(9) Uani 0.921(4) 1 d D U P A 2
C13 C 0.6084(3) 0.7001(2) 0.90261(19) 0.0283(5) Uani 1 1 d . U . . .
F1 F 0.6526(2) 0.60273(13) 0.89916(12) 0.0410(4) Uani 1 1 d . U . . .
F2 F 0.5602(2) 0.71142(14) 0.97315(12) 0.0450(5) Uani 1 1 d . U . . .
F3 F 0.49446(18) 0.71263(14) 0.84409(12) 0.0398(4) Uani 1 1 d . U . . .
O3 O 0.8602(2) 0.76684(18) 0.96085(15) 0.0464(6) Uani 1 1 d . U . . .
O4 O 0.6818(2) 0.88874(16) 0.89574(13) 0.0367(5) Uani 1 1 d . U . . .
O5 O 0.7890(3) 0.76498(17) 0.81469(14) 0.0420(5) Uani 1 1 d . U . . .
S1 S 0.75231(8) 0.79005(6) 0.89229(5) 0.02808(16) Uani 1 1 d . 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
C1 C2 1.507(4) . ?
C1 N2 1.510(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.486(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.490(4) . ?
C3 C4 1.506(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.508(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.508(4) . ?
C5 C6 1.522(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.504(4) . ?
C7 C8 1.514(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.506(4) . ?
C9 C10 1.524(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.505(4) . ?
C11 C12 1.509(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.076(2) . ?
N3 Pt1 2.004(2) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.074(2) . ?
Pt1 O1A 2.047(2) . ?
Pt1 N1 2.047(2) . ?
N1 O1 1.178(9) . ?
N1 O2 1.206(10) . ?
N1A O2A 1.207(4) . ?
N1A O1A 1.325(3) . ?
C13 F1 1.333(3) . ?
C13 F3 1.336(3) . ?
C13 F2 1.338(3) . ?
C13 S1 1.808(3) . ?
O3 S1 1.433(2) . ?
O4 S1 1.445(2) . ?
O5 S1 1.433(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 N2 110.3(2) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.9(2) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.1(2) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 109.5(2) . . ?
C3 C4 H4A 109.8 . . ?
N4 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
N4 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 116.8(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 114.0(2) . . ?
N2 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 116.7(2) . . ?
N4 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N4 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 113.9(3) . . ?
N4 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N4 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 N2 C5 109.3(2) . . ?
C7 N2 C1 110.3(2) . . ?
C5 N2 C1 110.1(2) . . ?
C7 N2 Pt1 115.77(19) . . ?
C5 N2 Pt1 105.24(17) . . ?
C1 N2 Pt1 105.94(17) . . ?
C2 N3 C3 115.8(2) . . ?
C2 N3 Pt1 107.64(17) . . ?
C3 N3 Pt1 107.00(17) . . ?
C2 N3 H3 108.8 . . ?
C3 N3 H3 108.8 . . ?
Pt1 N3 H3 108.8 . . ?
C11 N4 C9 108.9(2) . . ?
C11 N4 C4 110.2(2) . . ?
C9 N4 C4 110.4(2) . . ?
C11 N4 Pt1 115.8(2) . . ?
C9 N4 Pt1 105.99(17) . . ?
C4 N4 Pt1 105.54(17) . . ?
N3 Pt1 O1A 173.94(9) . . ?
N3 Pt1 N1 173.94(9) . . ?
N3 Pt1 N4 85.56(9) . . ?
O1A Pt1 N4 93.66(9) . . ?
N1 Pt1 N4 93.66(9) . . ?
N3 Pt1 N2 85.14(9) . . ?
O1A Pt1 N2 94.73(9) . . ?
N1 Pt1 N2 94.73(9) . . ?
N4 Pt1 N2 167.61(10) . . ?
O1 N1 O2 123.6(14) . . ?
O1 N1 Pt1 122.6(11) . . ?
O2 N1 Pt1 113.8(15) . . ?
O2A N1A O1A 114.0(3) . . ?
N1A O1A Pt1 123.4(2) . . ?
F1 C13 F3 107.4(2) . . ?
F1 C13 F2 107.0(2) . . ?
F3 C13 F2 107.1(2) . . ?
F1 C13 S1 111.6(2) . . ?
F3 C13 S1 111.5(2) . . ?
F2 C13 S1 111.9(2) . . ?
O3 S1 O5 116.14(15) . . ?
O3 S1 O4 114.84(14) . . ?
O5 S1 O4 114.42(14) . . ?
O3 S1 C13 102.98(14) . . ?
O5 S1 C13 103.19(14) . . ?
O4 S1 C13 102.66(14) . . ?

_refine_diff_density_max         0.662
_refine_diff_density_min         -1.001
_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_Pt_MS3h_100K
_database_code_depnum_ccdc_archive 'CCDC 1564464'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3067(4)
_cell_length_b                   13.0046(5)
_cell_length_c                   16.7285(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.001(4)
_cell_angle_gamma                90
_cell_volume                     1999.72(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3307
_cell_measurement_theta_min      3.8850
_cell_measurement_theta_max      29.2710

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.077
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.1049
0 0 1 0.1049
0 1 1 0.1829
0 -1 -1 0.1387
-1 5 1 0.2564
1 -5 1 0.2321
-1 0 1 0.0383
1 0 -1 0.0383
5 1 0 0.0756
5 4 2 0.0934
3 2 -5 0.0800
_exptl_absorpt_coefficient_mu    7.180
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            9264
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.367
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4085
_reflns_number_gt                3338
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0418P)²+1.0127P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4085
_refine_ls_number_parameters     257
_refine_ls_number_restraints     280
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0854
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.022
_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 0.5116(7) 0.5635(5) 0.1851(4) 0.0288(12) Uani 1 1 d . U . . .
H1A H 0.6028 0.5543 0.1623 0.035 Uiso 1 1 calc R U . . .
H1B H 0.4591 0.6232 0.1579 0.035 Uiso 1 1 calc R U . . .
C2 C 0.5478(7) 0.5845(5) 0.2743(4) 0.0302(12) Uani 1 1 d . U . . .
H2A H 0.6115 0.5299 0.3016 0.036 Uiso 1 1 calc R U . . .
H2B H 0.5981 0.6515 0.2841 0.036 Uiso 1 1 calc R U . . .
C3 C 0.4115(7) 0.5844(5) 0.3937(4) 0.0318(13) Uani 1 1 d . U . . .
H3A H 0.4463 0.6513 0.4176 0.038 Uiso 1 1 calc R U . . .
H3B H 0.4783 0.5298 0.4183 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2583(7) 0.5635(5) 0.4087(4) 0.0313(12) Uani 1 1 d . U . . .
H4A H 0.2572 0.5566 0.4676 0.038 Uiso 1 1 calc R U . . .
H4B H 0.1942 0.6216 0.3883 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3394(7) 0.4689(5) 0.0842(4) 0.0307(12) Uani 1 1 d . U . . .
H5A H 0.2948 0.4005 0.0717 0.037 Uiso 1 1 calc R U . . .
H5B H 0.4106 0.4804 0.0468 0.037 Uiso 1 1 calc R U . . .
C6 C 0.2211(8) 0.5504(5) 0.0683(4) 0.0378(16) Uani 1 1 d . U . . .
H6A H 0.1703 0.5438 0.0126 0.057 Uiso 1 1 calc R U . . .
H6B H 0.2652 0.6189 0.0759 0.057 Uiso 1 1 calc R U . . .
H6C H 0.1517 0.5411 0.1061 0.057 Uiso 1 1 calc R U . . .
C7 C 0.5151(7) 0.3727(5) 0.1810(4) 0.0317(13) Uani 1 1 d . U . . .
H7A H 0.5720 0.3759 0.2362 0.038 Uiso 1 1 calc R U . . .
H7B H 0.4515 0.3114 0.1789 0.038 Uiso 1 1 calc R U . . .
C8 C 0.6199(7) 0.3570(5) 0.1218(4) 0.0403(16) Uani 1 1 d . U . . .
H8A H 0.5653 0.3482 0.0672 0.060 Uiso 1 1 calc R U . . .
H8B H 0.6789 0.2956 0.1369 0.060 Uiso 1 1 calc R U . . .
H8C H 0.6837 0.4172 0.1227 0.060 Uiso 1 1 calc R U . . .
C9 C 0.0396(7) 0.4614(5) 0.3570(4) 0.0323(13) Uani 1 1 d . U . . .
H9A H 0.0072 0.3923 0.3368 0.039 Uiso 1 1 calc R U . . .
H9B H 0.0096 0.4705 0.4108 0.039 Uiso 1 1 calc R U . . .
C10 C -0.0351(8) 0.5406(6) 0.3005(5) 0.052(2) Uani 1 1 d . U . . .
H10A H -0.0018 0.5348 0.2479 0.078 Uiso 1 1 calc R U . . .
H10B H -0.0119 0.6093 0.3230 0.078 Uiso 1 1 calc R U . . .
H10C H -0.1405 0.5297 0.2935 0.078 Uiso 1 1 calc R U . . .
C11 C 0.2659(6) 0.3748(5) 0.4155(4) 0.0298(12) Uani 1 1 d . U . . .
H11A H 0.2393 0.3120 0.3831 0.036 Uiso 1 1 calc R U . . .
H11B H 0.3732 0.3806 0.4235 0.036 Uiso 1 1 calc R U . . .
C12 C 0.2199(7) 0.3601(5) 0.4973(4) 0.0362(15) Uani 1 1 d . U . . .
H12A H 0.1143 0.3506 0.4905 0.054 Uiso 1 1 calc R U . . .
H12B H 0.2473 0.4209 0.5309 0.054 Uiso 1 1 calc R U . . .
H12C H 0.2684 0.2993 0.5236 0.054 Uiso 1 1 calc R U . . .
N2 N 0.4183(6) 0.4680(4) 0.1685(3) 0.0274(9) Uani 1 1 d . U . . .
N3 N 0.4059(5) 0.5862(4) 0.3048(3) 0.0281(10) Uani 1 1 d . U . . .
H3 H 0.3517 0.6493 0.2831 0.034 Uiso 1 1 calc R U . . .
N4 N 0.2031(5) 0.4663(3) 0.3664(3) 0.0237(8) Uani 1 1 d . U . . .
Pt1 Pt 0.29133(2) 0.46279(2) 0.25995(2) 0.02233(9) Uani 1 1 d . U . . .
N1 N 0.1850(3) 0.3306(3) 0.21956(13) 0.0335(9) Uani 0.321(8) 1 d D U P A 1
O1 O 0.2345(7) 0.2510(8) 0.2416(3) 0.056(2) Uani 0.321(8) 1 d D U P A 1
O2 O 0.0720(8) 0.3408(12) 0.1732(3) 0.056(2) Uani 0.321(8) 1 d D U P A 1
N1A N 0.0633(7) 0.3209(7) 0.1701(3) 0.0335(9) Uani 0.562(9) 1 d D U P A 2
O1A O 0.1850(3) 0.3306(3) 0.21956(13) 0.0335(9) Uani 0.562(9) 1 d D U P A 2
O2A O 0.0120(7) 0.4084(6) 0.1471(4) 0.056(2) Uani 0.562(9) 1 d D U P A 2
O1B O 0.1850(3) 0.3306(3) 0.21956(13) 0.0335(9) Uani 0.116(9) 1 d D U P A 3
N1B N 0.0738(11) 0.3716(17) 0.1732(5) 0.0335(9) Uani 0.116(9) 1 d D U P A 3
O2B O -0.0099(11) 0.298(2) 0.1407(5) 0.056(2) Uani 0.116(9) 1 d D U P A 3
C13 C 0.6081(6) 0.1981(4) 0.4034(4) 0.0277(9) Uani 1 1 d . U . . .
F1 F 0.6542(4) 0.1005(3) 0.3997(2) 0.0331(8) Uani 1 1 d . U . . .
F2 F 0.4946(3) 0.2100(3) 0.3447(2) 0.0334(8) Uani 1 1 d . U . . .
F3 F 0.5593(4) 0.2091(3) 0.4736(2) 0.0371(8) Uani 1 1 d . U . . .
O3 O 0.7904(4) 0.2642(3) 0.3153(3) 0.0350(9) Uani 1 1 d . U . . .
O4 O 0.6805(4) 0.3872(3) 0.3962(3) 0.0319(9) Uani 1 1 d . U . . .
O5 O 0.8603(4) 0.2648(3) 0.4613(3) 0.0382(10) Uani 1 1 d . U . . .
S1 S 0.75259(15) 0.28836(11) 0.39296(10) 0.0271(3) Uani 1 1 d . 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
C1 C2 1.502(9) . ?
C1 N2 1.517(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.488(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.481(8) . ?
C3 C4 1.511(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.499(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.485(8) . ?
C5 C6 1.522(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.510(8) . ?
C7 N2 1.527(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.494(9) . ?
C9 N4 1.507(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.508(8) . ?
C11 N4 1.511(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.075(5) . ?
N3 Pt1 2.006(5) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.075(5) . ?
Pt1 O1B 2.045(4) . ?
Pt1 O1A 2.045(4) . ?
Pt1 N1 2.045(4) . ?
N1 O1 1.169(8) . ?
N1 O2 1.213(8) . ?
N1A O2A 1.270(8) . ?
N1A O1A 1.301(7) . ?
O1B N1B 1.306(10) . ?
N1B O2B 1.298(10) . ?
C13 F3 1.332(7) . ?
C13 F2 1.335(7) . ?
C13 F1 1.343(7) . ?
C13 S1 1.814(6) . ?
O3 S1 1.433(5) . ?
O4 S1 1.455(4) . ?
O5 S1 1.431(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 111.3(5) . . ?
C2 C1 H1A 109.4 . . ?
N2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 105.7(5) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 106.5(5) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 109.6(5) . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 114.1(5) . . ?
N2 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N2 116.6(5) . . ?
C8 C7 H7A 108.2 . . ?
N2 C7 H7A 108.2 . . ?
C8 C7 H7B 108.2 . . ?
N2 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N4 113.5(5) . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
N4 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 116.9(5) . . ?
C12 C11 H11A 108.1 . . ?
N4 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
N4 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C1 110.5(5) . . ?
C5 N2 C7 109.3(4) . . ?
C1 N2 C7 109.3(5) . . ?
C5 N2 Pt1 116.6(4) . . ?
C1 N2 Pt1 105.5(3) . . ?
C7 N2 Pt1 105.3(3) . . ?
C3 N3 C2 116.7(5) . . ?
C3 N3 Pt1 107.2(4) . . ?
C2 N3 Pt1 108.0(4) . . ?
C3 N3 H3 108.2 . . ?
C2 N3 H3 108.2 . . ?
Pt1 N3 H3 108.2 . . ?
C4 N4 C9 110.6(4) . . ?
C4 N4 C11 109.4(5) . . ?
C9 N4 C11 108.8(4) . . ?
C4 N4 Pt1 105.8(3) . . ?
C9 N4 Pt1 116.0(4) . . ?
C11 N4 Pt1 106.1(3) . . ?
N3 Pt1 O1B 175.91(18) . . ?
N3 Pt1 O1A 175.91(18) . . ?
N3 Pt1 N1 175.91(18) . . ?
N3 Pt1 N4 85.42(19) . . ?
O1B Pt1 N4 93.80(14) . . ?
O1A Pt1 N4 93.80(14) . . ?
N1 Pt1 N4 93.80(14) . . ?
N3 Pt1 N2 85.35(19) . . ?
O1B Pt1 N2 94.90(15) . . ?
O1A Pt1 N2 94.90(15) . . ?
N1 Pt1 N2 94.90(15) . . ?
N4 Pt1 N2 168.35(19) . . ?
O1 N1 O2 123.9(9) . . ?
O1 N1 Pt1 119.6(4) . . ?
O2 N1 Pt1 116.5(8) . . ?
O2A N1A O1A 110.7(7) . . ?
N1A O1A Pt1 128.4(5) . . ?
N1B O1B Pt1 98.7(10) . . ?
O2B N1B O1B 108.5(11) . . ?
F3 C13 F2 107.3(5) . . ?
F3 C13 F1 107.3(5) . . ?
F2 C13 F1 107.3(5) . . ?
F3 C13 S1 112.1(4) . . ?
F2 C13 S1 111.5(4) . . ?
F1 C13 S1 111.1(4) . . ?
O5 S1 O3 115.9(3) . . ?
O5 S1 O4 115.4(3) . . ?
O3 S1 O4 114.1(3) . . ?
O5 S1 C13 102.8(3) . . ?
O3 S1 C13 103.6(3) . . ?
O4 S1 C13 102.4(3) . . ?

_refine_diff_density_max         2.044
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.176

####################################################################### 
# 
# 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_Pt_MS3h_200K
_database_code_depnum_ccdc_archive 'CCDC 1564473'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3268(2)
_cell_length_b                   12.9755(3)
_cell_length_c                   16.7508(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.170(2)
_cell_angle_gamma                90
_cell_volume                     2001.27(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    10095
_cell_measurement_theta_min      3.9810
_cell_measurement_theta_max      29.5970

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 5 0.1067
0 3 -5 0.1696
-3 5 2 0.1520
-3 -5 2 0.1832
-5 1 4 0.0508
0 -1 1 0.1437
-1 0 -5 0.1033
-1 -5 -3 0.2517
-1 1 -5 0.1103
1 5 -1 0.2318
-5 0 4 0.0512
5 0 -4 0.0348
_exptl_absorpt_coefficient_mu    7.174
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            21907
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.373
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4086
_reflns_number_gt                3663
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0194P)²+0.7593P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4086
_refine_ls_number_parameters     255
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0429
_refine_ls_wR_factor_gt          0.0412
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.003
_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 -0.0069(4) 0.5641(2) 0.8173(2) 0.0302(6) Uani 1 1 d . U . . .
H1A H -0.0978 0.5552 0.8401 0.036 Uiso 1 1 calc R U . . .
H1B H 0.0465 0.6236 0.8447 0.036 Uiso 1 1 calc R U . . .
C2 C -0.0426(3) 0.5849(2) 0.72773(19) 0.0289(6) Uani 1 1 d . U . . .
H2A H -0.1052 0.5296 0.7004 0.035 Uiso 1 1 calc R U . . .
H2B H -0.0938 0.6516 0.7176 0.035 Uiso 1 1 calc R U . . .
C3 C 0.0902(3) 0.5850(2) 0.60801(18) 0.0297(6) Uani 1 1 d . U . . .
H3A H 0.0543 0.6516 0.5839 0.036 Uiso 1 1 calc R U . . .
H3B H 0.0237 0.5296 0.5843 0.036 Uiso 1 1 calc R U . . .
C4 C 0.2428(4) 0.5644(2) 0.5928(2) 0.0312(7) Uani 1 1 d . U . . .
H4A H 0.2433 0.5578 0.5339 0.037 Uiso 1 1 calc R U . . .
H4B H 0.3066 0.6228 0.6132 0.037 Uiso 1 1 calc R U . . .
C5 C -0.0091(3) 0.3732(2) 0.81955(19) 0.0287(6) Uani 1 1 d . U . . .
H5A H 0.0551 0.3121 0.8225 0.034 Uiso 1 1 calc R U . . .
H5B H -0.0646 0.3759 0.7640 0.034 Uiso 1 1 calc R U . . .
C6 C -0.1164(4) 0.3567(3) 0.8779(2) 0.0421(8) Uani 1 1 d . U . . .
H6A H -0.1759 0.2957 0.8615 0.063 Uiso 1 1 calc R U . . .
H6B H -0.1793 0.4173 0.8772 0.063 Uiso 1 1 calc R U . . .
H6C H -0.0631 0.3464 0.9327 0.063 Uiso 1 1 calc R U . . .
C7 C 0.1660(4) 0.4680(2) 0.91776(19) 0.0300(7) Uani 1 1 d . U . . .
H7A H 0.2142 0.4004 0.9290 0.036 Uiso 1 1 calc R U . . .
H7B H 0.0952 0.4763 0.9555 0.036 Uiso 1 1 calc R U . . .
C8 C 0.2795(4) 0.5523(3) 0.9344(2) 0.0382(8) Uani 1 1 d . U . . .
H8A H 0.3444 0.5492 0.8939 0.057 Uiso 1 1 calc R U . . .
H8B H 0.3360 0.5425 0.9884 0.057 Uiso 1 1 calc R U . . .
H8C H 0.2314 0.6196 0.9318 0.057 Uiso 1 1 calc R U . . .
C9 C 0.2365(3) 0.3743(2) 0.58731(18) 0.0290(6) Uani 1 1 d . U . . .
H9A H 0.1293 0.3789 0.5803 0.035 Uiso 1 1 calc R U . . .
H9B H 0.2656 0.3120 0.6200 0.035 Uiso 1 1 calc R U . . .
C10 C 0.2804(4) 0.3593(3) 0.5041(2) 0.0372(8) Uani 1 1 d . U . . .
H10A H 0.2537 0.4207 0.4709 0.056 Uiso 1 1 calc R U . . .
H10B H 0.2301 0.2990 0.4778 0.056 Uiso 1 1 calc R U . . .
H10C H 0.3856 0.3486 0.5101 0.056 Uiso 1 1 calc R U . . .
C11 C 0.4614(3) 0.4633(2) 0.6437(2) 0.0328(7) Uani 1 1 d . U . . .
H11A H 0.4899 0.4692 0.5895 0.039 Uiso 1 1 calc R U . . .
H11B H 0.4952 0.3954 0.6663 0.039 Uiso 1 1 calc R U . . .
C12 C 0.5371(4) 0.5468(3) 0.6974(3) 0.0492(10) Uani 1 1 d . U . . .
H12A H 0.5287 0.6124 0.6681 0.074 Uiso 1 1 calc R U . . .
H12B H 0.6399 0.5290 0.7128 0.074 Uiso 1 1 calc R U . . .
H12C H 0.4918 0.5531 0.7461 0.074 Uiso 1 1 calc R U . . .
N2 N 0.0851(3) 0.46780(17) 0.83240(15) 0.0230(5) Uani 1 1 d . U . . .
N3 N 0.0991(3) 0.58769(18) 0.69749(14) 0.0233(5) Uani 1 1 d . U . . .
H3 H 0.1530 0.6511 0.7187 0.028 Uiso 1 1 calc R U . . .
N4 N 0.2988(3) 0.46696(17) 0.63484(15) 0.0235(5) Uani 1 1 d . U . . .
Pt1 Pt 0.21285(2) 0.46378(2) 0.74170(2) 0.01902(5) Uani 1 1 d . U . . .
N1 N 0.3130(2) 0.32812(15) 0.77962(13) 0.0295(5) Uani 0.072(4) 1 d D U P A 1
O1 O 0.280(3) 0.2478(12) 0.7483(14) 0.0295(5) Uani 0.072(4) 1 d D U P A 1
O2 O 0.406(3) 0.337(2) 0.8378(15) 0.0295(5) Uani 0.072(4) 1 d D U P A 1
N1A N 0.4400(3) 0.3230(3) 0.8280(2) 0.0396(9) Uani 0.928(4) 1 d D U P A 2
O1A O 0.3130(2) 0.32812(15) 0.77962(13) 0.0295(5) Uani 0.928(4) 1 d D U P A 2
O2A O 0.4899(3) 0.4060(2) 0.84953(18) 0.0542(9) Uani 0.928(4) 1 d D U P A 2
C13 C 0.6084(3) 0.7001(2) 0.90258(19) 0.0283(5) Uani 1 1 d . U . . .
F1 F 0.6524(2) 0.60270(13) 0.89920(12) 0.0415(5) Uani 1 1 d . U . . .
F2 F 0.5601(2) 0.71166(14) 0.97310(12) 0.0455(5) Uani 1 1 d . U . . .
F3 F 0.49443(19) 0.71256(14) 0.84439(12) 0.0401(5) Uani 1 1 d . U . . .
O3 O 0.8603(2) 0.76689(19) 0.96081(16) 0.0470(6) Uani 1 1 d . U . . .
O4 O 0.6818(2) 0.88893(16) 0.89558(13) 0.0368(5) Uani 1 1 d . U . . .
O5 O 0.7892(3) 0.76490(17) 0.81470(15) 0.0420(6) Uani 1 1 d . U . . .
S1 S 0.75226(8) 0.79011(6) 0.89227(5) 0.02819(17) Uani 1 1 d . 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
C1 C2 1.509(4) . ?
C1 N2 1.514(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.489(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.488(4) . ?
C3 C4 1.509(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.501(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.506(4) . ?
C5 C6 1.521(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N2 1.506(4) . ?
C7 C8 1.516(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.506(4) . ?
C9 C10 1.527(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N4 1.501(4) . ?
C11 C12 1.509(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 Pt1 2.075(2) . ?
N3 Pt1 2.002(2) . ?
N3 H3 1.0000 . ?
N4 Pt1 2.075(2) . ?
Pt1 O1A 2.046(2) . ?
Pt1 N1 2.046(2) . ?
N1 O1 1.185(9) . ?
N1 O2 1.204(10) . ?
N1A O2A 1.205(4) . ?
N1A O1A 1.326(3) . ?
C13 F1 1.332(3) . ?
C13 F3 1.333(3) . ?
C13 F2 1.338(4) . ?
C13 S1 1.808(3) . ?
O3 S1 1.434(2) . ?
O4 S1 1.446(2) . ?
O5 S1 1.434(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 N2 110.0(2) . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.0(2) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.8(2) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 109.7(2) . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 116.8(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 113.9(3) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 116.6(3) . . ?
N4 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N4 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 113.9(3) . . ?
N4 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N4 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 N2 C7 109.3(2) . . ?
C5 N2 C1 110.3(2) . . ?
C7 N2 C1 109.9(2) . . ?
C5 N2 Pt1 105.37(17) . . ?
C7 N2 Pt1 115.84(19) . . ?
C1 N2 Pt1 105.95(17) . . ?
C3 N3 C2 115.6(2) . . ?
C3 N3 Pt1 107.13(17) . . ?
C2 N3 Pt1 107.53(17) . . ?
C3 N3 H3 108.8 . . ?
C2 N3 H3 108.8 . . ?
Pt1 N3 H3 108.8 . . ?
C4 N4 C11 110.1(2) . . ?
C4 N4 C9 110.4(3) . . ?
C11 N4 C9 109.0(2) . . ?
C4 N4 Pt1 105.56(17) . . ?
C11 N4 Pt1 115.9(2) . . ?
C9 N4 Pt1 105.70(17) . . ?
N3 Pt1 O1A 174.04(9) . . ?
N3 Pt1 N1 174.04(9) . . ?
N3 Pt1 N4 85.40(9) . . ?
O1A Pt1 N4 93.72(9) . . ?
N1 Pt1 N4 93.72(9) . . ?
N3 Pt1 N2 85.32(9) . . ?
O1A Pt1 N2 94.67(9) . . ?
N1 Pt1 N2 94.67(9) . . ?
N4 Pt1 N2 167.63(10) . . ?
O1 N1 O2 122.9(13) . . ?
O1 N1 Pt1 123.0(12) . . ?
O2 N1 Pt1 114.0(14) . . ?
O2A N1A O1A 113.8(3) . . ?
N1A O1A Pt1 123.5(2) . . ?
F1 C13 F3 107.4(2) . . ?
F1 C13 F2 107.1(2) . . ?
F3 C13 F2 106.9(2) . . ?
F1 C13 S1 111.8(2) . . ?
F3 C13 S1 111.7(2) . . ?
F2 C13 S1 111.8(2) . . ?
O3 S1 O5 115.96(15) . . ?
O3 S1 O4 114.93(14) . . ?
O5 S1 O4 114.41(14) . . ?
O3 S1 C13 103.02(14) . . ?
O5 S1 C13 103.19(14) . . ?
O4 S1 C13 102.76(14) . . ?

_refine_diff_density_max         0.725
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.093

####################################################################### 
# 
# 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_Pt_GS_200K
_database_code_depnum_ccdc_archive 'CCDC 1564471'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2636(3)
_cell_length_b                   13.1409(4)
_cell_length_c                   17.1074(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.567(3)
_cell_angle_gamma                90
_cell_volume                     2068.85(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    7771
_cell_measurement_theta_min      3.8910
_cell_measurement_theta_max      29.6150

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 5 0.1067
-1 0 -5 0.1033
-1 1 -5 0.1103
1 5 -1 0.2318
0 3 -5 0.1696
0 -1 1 0.1437
-1 -5 -3 0.2517
5 0 -4 0.0348
-5 0 4 0.0512
-5 1 4 0.0508
-3 -5 2 0.1832
-3 5 2 0.1520
_exptl_absorpt_coefficient_mu    6.940
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            17464
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.441
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_full        25.242
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4226
_reflns_number_gt                3722
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0202P)²+0.8181P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4226
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0487
_refine_ls_wR_factor_gt          0.0461
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_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 0.7413(4) 0.4371(3) 0.5927(2) 0.0315(8) Uani 1 1 d . . . . .
H1A H 0.7511 0.4390 0.5369 0.038 Uiso 1 1 calc R U . . .
H1B H 0.8028 0.3829 0.6162 0.038 Uiso 1 1 calc R U . . .
C2 C 0.5860(4) 0.4159(3) 0.6044(2) 0.0299(8) Uani 1 1 d . . . . .
H2A H 0.5221 0.4663 0.5774 0.036 Uiso 1 1 calc R U . . .
H2B H 0.5571 0.3490 0.5843 0.036 Uiso 1 1 calc R U . . .
C3 C 0.4348(4) 0.4234(3) 0.7183(2) 0.0293(8) Uani 1 1 d . . . . .
H3A H 0.3857 0.3586 0.7087 0.035 Uiso 1 1 calc R U . . .
H3B H 0.3752 0.4764 0.6916 0.035 Uiso 1 1 calc R U . . .
C4 C 0.4618(4) 0.4449(3) 0.8056(2) 0.0328(9) Uani 1 1 d . . . . .
H4A H 0.3697 0.4535 0.8267 0.039 Uiso 1 1 calc R U . . .
H4B H 0.5120 0.3876 0.8323 0.039 Uiso 1 1 calc R U . . .
C5 C 0.7303(4) 0.6240(3) 0.5772(2) 0.0319(8) Uani 1 1 d . . . . .
H5A H 0.6253 0.6176 0.5689 0.038 Uiso 1 1 calc R U . . .
H5B H 0.7525 0.6875 0.6050 0.038 Uiso 1 1 calc R U . . .
C6 C 0.7862(4) 0.6309(3) 0.4976(2) 0.0452(10) Uani 1 1 d . . . . .
H6A H 0.7382 0.6858 0.4681 0.068 Uiso 1 1 calc R U . . .
H6B H 0.7669 0.5682 0.4697 0.068 Uiso 1 1 calc R U . . .
H6C H 0.8890 0.6432 0.5047 0.068 Uiso 1 1 calc R U . . .
C7 C 0.9509(4) 0.5426(3) 0.6415(2) 0.0393(10) Uani 1 1 d . . . . .
H7A H 0.9796 0.6121 0.6542 0.047 Uiso 1 1 calc R U . . .
H7B H 0.9877 0.5252 0.5923 0.047 Uiso 1 1 calc R U . . .
C8 C 1.0217(5) 0.4732(4) 0.7055(3) 0.0581(13) Uani 1 1 d . . . . .
H8A H 0.9968 0.4038 0.6926 0.087 Uiso 1 1 calc R U . . .
H8B H 0.9878 0.4905 0.7547 0.087 Uiso 1 1 calc R U . . .
H8C H 1.1253 0.4812 0.7096 0.087 Uiso 1 1 calc R U . . .
C9 C 0.6281(5) 0.5376(3) 0.9034(2) 0.0398(10) Uani 1 1 d . . . . .
H9A H 0.5575 0.5211 0.9391 0.048 Uiso 1 1 calc R U . . .
H9B H 0.6660 0.6049 0.9170 0.048 Uiso 1 1 calc R U . . .
C10 C 0.7511(5) 0.4618(3) 0.9149(3) 0.0508(12) Uani 1 1 d . . . . .
H10A H 0.8218 0.4776 0.8798 0.076 Uiso 1 1 calc R U . . .
H10B H 0.7139 0.3945 0.9039 0.076 Uiso 1 1 calc R U . . .
H10C H 0.7960 0.4650 0.9683 0.076 Uiso 1 1 calc R U . . .
C11 C 0.4565(4) 0.6332(3) 0.8092(2) 0.0372(9) Uani 1 1 d . . . . .
H11A H 0.4049 0.6310 0.7566 0.045 Uiso 1 1 calc R U . . .
H11B H 0.5184 0.6930 0.8122 0.045 Uiso 1 1 calc R U . . .
C12 C 0.3457(6) 0.6466(4) 0.8672(3) 0.0641(15) Uani 1 1 d . . . . .
H12A H 0.2904 0.7074 0.8547 0.096 Uiso 1 1 calc R U . . .
H12B H 0.3950 0.6519 0.9196 0.096 Uiso 1 1 calc R U . . .
H12C H 0.2816 0.5890 0.8642 0.096 Uiso 1 1 calc R U . . .
C13 C 0.3893(4) 0.8110(3) 0.5878(2) 0.0343(9) Uani 1 1 d . . . . .
F1 F 0.3417(3) 0.90591(16) 0.59078(15) 0.0531(6) Uani 1 1 d . . . . .
F2 F 0.4442(3) 0.79960(19) 0.52008(15) 0.0593(7) Uani 1 1 d . . . . .
F3 F 0.4988(3) 0.8007(2) 0.64454(16) 0.0583(7) Uani 1 1 d . . . . .
N2 N 0.7899(3) 0.53733(19) 0.62974(17) 0.0244(6) Uani 1 1 d . . . . .
N3 N 0.5797(3) 0.42088(19) 0.69012(16) 0.0205(6) Uani 1 1 d . . . . .
H3 H 0.6311 0.3612 0.7137 0.025 Uiso 1 1 calc R U . . .
N4 N 0.5524(3) 0.54003(19) 0.82049(17) 0.0277(7) Uani 1 1 d . . . . .
O3 O 0.2051(3) 0.7427(2) 0.67514(17) 0.0495(8) Uani 1 1 d . . . . .
O4 O 0.1417(3) 0.7399(2) 0.53317(19) 0.0593(9) Uani 1 1 d . . . . .
O5 O 0.3213(3) 0.62295(18) 0.59535(16) 0.0414(6) Uani 1 1 d . . . . .
Pt1 Pt 0.68923(2) 0.54516(2) 0.73216(2) 0.01990(5) Uani 1 1 d . . . . .
S002 S 0.24691(10) 0.71897(7) 0.59926(6) 0.0330(2) Uani 1 1 d . . . . .
N1 N 0.7963(3) 0.6706(2) 0.77285(18) 0.0329(7) Uani 1 1 d . . . . .
O1 O 0.8937(5) 0.6692(3) 0.8267(2) 0.0989(16) Uani 1 1 d . . . . .
O2 O 0.7691(4) 0.7515(2) 0.7419(2) 0.0801(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
C1 C2 1.501(5) . ?
C1 N2 1.508(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.476(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.477(4) . ?
C3 C4 1.513(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.511(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.514(5) . ?
C5 N2 1.515(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.484(5) . ?
C7 C8 1.516(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.508(5) . ?
C9 C10 1.510(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.513(4) . ?
C11 C12 1.517(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 F1 1.326(4) . ?
C13 F2 1.326(4) . ?
C13 F3 1.328(4) . ?
C13 S002 1.816(4) . ?
N2 Pt1 2.079(3) . ?
N3 Pt1 2.012(3) . ?
N3 H3 0.9800 . ?
N4 Pt1 2.082(3) . ?
O3 S002 1.431(3) . ?
O4 S002 1.432(3) . ?
O5 S002 1.443(3) . ?
Pt1 N1 2.007(3) . ?
N1 O2 1.202(4) . ?
N1 O1 1.213(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 110.5(3) . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.8(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.8(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.3(3) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 N2 116.1(3) . . ?
C6 C5 H5A 108.3 . . ?
N2 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
N2 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 114.5(3) . . ?
N2 C7 H7A 108.6 . . ?
C8 C7 H7A 108.6 . . ?
N2 C7 H7B 108.6 . . ?
C8 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 113.5(3) . . ?
N4 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N4 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 116.2(3) . . ?
N4 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
F1 C13 F2 107.5(3) . . ?
F1 C13 F3 107.3(3) . . ?
F2 C13 F3 106.8(3) . . ?
F1 C13 S002 112.0(3) . . ?
F2 C13 S002 112.0(3) . . ?
F3 C13 S002 110.9(3) . . ?
C7 N2 C1 110.1(3) . . ?
C7 N2 C5 109.7(3) . . ?
C1 N2 C5 109.7(3) . . ?
C7 N2 Pt1 115.1(2) . . ?
C1 N2 Pt1 104.85(19) . . ?
C5 N2 Pt1 107.1(2) . . ?
C2 N3 C3 117.8(3) . . ?
C2 N3 Pt1 108.40(19) . . ?
C3 N3 Pt1 107.8(2) . . ?
C2 N3 H3 107.5 . . ?
C3 N3 H3 107.5 . . ?
Pt1 N3 H3 107.5 . . ?
C9 N4 C4 109.3(3) . . ?
C9 N4 C11 109.9(3) . . ?
C4 N4 C11 110.0(3) . . ?
C9 N4 Pt1 115.3(2) . . ?
C4 N4 Pt1 106.1(2) . . ?
C11 N4 Pt1 106.2(2) . . ?
N1 Pt1 N3 179.05(12) . . ?
N1 Pt1 N2 94.67(11) . . ?
N3 Pt1 N2 85.13(10) . . ?
N1 Pt1 N4 95.32(11) . . ?
N3 Pt1 N4 84.79(11) . . ?
N2 Pt1 N4 168.27(12) . . ?
O3 S002 O4 116.4(2) . . ?
O3 S002 O5 114.40(16) . . ?
O4 S002 O5 114.62(18) . . ?
O3 S002 C13 103.14(18) . . ?
O4 S002 C13 102.97(18) . . ?
O5 S002 C13 102.76(17) . . ?
O2 N1 O1 116.6(3) . . ?
O2 N1 Pt1 120.2(3) . . ?
O1 N1 Pt1 123.1(3) . . ?

_refine_diff_density_max         0.852
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.101

####################################################################### 
# 
# 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_Pt_VT_230K
_database_code_depnum_ccdc_archive 'CCDC 1564479'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3397(3)
_cell_length_b                   13.0157(4)
_cell_length_c                   16.8317(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.814(3)
_cell_angle_gamma                90
_cell_volume                     2021.94(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9247
_cell_measurement_theta_min      3.8930
_cell_measurement_theta_max      29.8160

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 5 0.1067
0 3 -5 0.1696
-3 5 2 0.1520
-3 -5 2 0.1832
-5 1 4 0.0508
0 -1 1 0.1437
-1 0 -5 0.1033
-1 -5 -3 0.2517
-1 1 -5 0.1103
1 5 -1 0.2318
-5 0 4 0.0512
5 0 -4 0.0348
_exptl_absorpt_coefficient_mu    7.101
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            22022
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.362
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4123
_reflns_number_gt                3611
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0224P)²+0.5083P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4123
_refine_ls_number_parameters     255
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0558
_refine_ls_wR_factor_gt          0.0532
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.073
_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 -0.0108(5) 0.5620(3) 0.8151(3) 0.0372(9) Uani 1 1 d . U . . .
H1A H -0.1002 0.5531 0.8371 0.045 Uiso 1 1 calc R U . . .
H1B H 0.0406 0.6202 0.8418 0.045 Uiso 1 1 calc R U . . .
C2 C -0.0453(5) 0.5831(3) 0.7265(3) 0.0353(9) Uani 1 1 d . U . . .
H2A H -0.1069 0.5294 0.6999 0.042 Uiso 1 1 calc R U . . .
H2B H -0.0950 0.6484 0.7170 0.042 Uiso 1 1 calc R U . . .
C3 C 0.0893(5) 0.5841(3) 0.6077(3) 0.0367(9) Uani 1 1 d . U . . .
H3A H 0.0549 0.6496 0.5846 0.044 Uiso 1 1 calc R U . . .
H3B H 0.0243 0.5305 0.5839 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2400(5) 0.5639(3) 0.5924(3) 0.0378(9) Uani 1 1 d . U . . .
H4A H 0.3021 0.6212 0.6119 0.045 Uiso 1 1 calc R U . . .
H4B H 0.2406 0.5572 0.5351 0.045 Uiso 1 1 calc R U . . .
C5 C -0.0133(5) 0.3725(3) 0.8183(3) 0.0365(9) Uani 1 1 d . U . . .
H5A H 0.0497 0.3129 0.8210 0.044 Uiso 1 1 calc R U . . .
H5B H -0.0674 0.3750 0.7643 0.044 Uiso 1 1 calc R U . . .
C6 C -0.1196(6) 0.3562(4) 0.8763(3) 0.0540(13) Uani 1 1 d . U . . .
H6A H -0.1752 0.2952 0.8617 0.081 Uiso 1 1 calc R U . . .
H6B H -0.1834 0.4142 0.8744 0.081 Uiso 1 1 calc R U . . .
H6C H -0.0677 0.3487 0.9298 0.081 Uiso 1 1 calc R U . . .
C7 C 0.1608(5) 0.4680(3) 0.9151(3) 0.0390(10) Uani 1 1 d . U . . .
H7A H 0.2064 0.4016 0.9266 0.047 Uiso 1 1 calc R U . . .
H7B H 0.0915 0.4776 0.9519 0.047 Uiso 1 1 calc R U . . .
C8 C 0.2759(6) 0.5509(3) 0.9309(3) 0.0494(12) Uani 1 1 d . U . . .
H8A H 0.3379 0.5477 0.8905 0.074 Uiso 1 1 calc R U . . .
H8B H 0.3323 0.5403 0.9829 0.074 Uiso 1 1 calc R U . . .
H8C H 0.2302 0.6171 0.9293 0.074 Uiso 1 1 calc R U . . .
C9 C 0.2366(5) 0.3748(3) 0.5863(3) 0.0367(9) Uani 1 1 d . U . . .
H9A H 0.1317 0.3790 0.5791 0.044 Uiso 1 1 calc R U . . .
H9B H 0.2646 0.3135 0.6176 0.044 Uiso 1 1 calc R U . . .
C10 C 0.2820(5) 0.3614(4) 0.5040(3) 0.0477(12) Uani 1 1 d . U . . .
H10A H 0.2593 0.4226 0.4728 0.072 Uiso 1 1 calc R U . . .
H10B H 0.2310 0.3042 0.4770 0.072 Uiso 1 1 calc R U . . .
H10C H 0.3844 0.3488 0.5102 0.072 Uiso 1 1 calc R U . . .
C11 C 0.4584(5) 0.4633(3) 0.6435(3) 0.0397(10) Uani 1 1 d . U . . .
H11A H 0.4870 0.4700 0.5908 0.048 Uiso 1 1 calc R U . . .
H11B H 0.4915 0.3967 0.6649 0.048 Uiso 1 1 calc R U . . .
C12 C 0.5334(6) 0.5458(4) 0.6976(4) 0.0612(15) Uani 1 1 d . U . . .
H12A H 0.5185 0.6113 0.6714 0.092 Uiso 1 1 calc R U . . .
H12B H 0.6353 0.5314 0.7089 0.092 Uiso 1 1 calc R U . . .
H12C H 0.4940 0.5473 0.7471 0.092 Uiso 1 1 calc R U . . .
N2 N 0.0806(4) 0.4670(2) 0.8306(2) 0.0298(7) Uani 1 1 d . U . . .
N3 N 0.0948(4) 0.5857(2) 0.69605(19) 0.0295(7) Uani 1 1 d . U . . .
H3 H 0.1472 0.6476 0.7171 0.035 Uiso 1 1 calc R U . . .
N4 N 0.2969(4) 0.4664(2) 0.6346(2) 0.0289(7) Uani 1 1 d . U . . .
Pt1 Pt 0.20950(2) 0.46284(2) 0.74029(2) 0.02456(6) Uani 1 1 d . U . . .
N1 N 0.3111(3) 0.3287(2) 0.77874(18) 0.0367(7) Uani 0.176(5) 1 d D U P A 1
O1 O 0.2698(15) 0.2506(9) 0.7506(8) 0.0367(7) Uani 0.176(5) 1 d D U P A 1
O2 O 0.4206(19) 0.3396(15) 0.8274(13) 0.0367(7) Uani 0.176(5) 1 d D U P A 1
N1A N 0.4354(7) 0.3206(5) 0.8276(5) 0.0647(19) Uani 0.824(5) 1 d D U P A 2
O1A O 0.3111(3) 0.3287(2) 0.77874(18) 0.0367(7) Uani 0.824(5) 1 d D U P A 2
O2A O 0.4866(5) 0.4046(3) 0.8481(3) 0.0694(15) Uani 0.824(5) 1 d D U P A 2
C13 C 0.6095(5) 0.6990(3) 0.9039(3) 0.0354(7) Uani 1 1 d . U . . .
F1 F 0.6540(3) 0.60206(18) 0.90068(17) 0.0513(7) Uani 1 1 d . U . . .
F2 F 0.5609(3) 0.7102(2) 0.97397(17) 0.0560(7) Uani 1 1 d . U . . .
F3 F 0.4968(3) 0.71103(19) 0.84606(17) 0.0512(7) Uani 1 1 d . U . . .
O3 O 0.8607(4) 0.7656(3) 0.9614(2) 0.0574(9) Uani 1 1 d . U . . .
O4 O 0.6830(3) 0.8869(2) 0.89719(19) 0.0458(8) Uani 1 1 d . U . . .
O5 O 0.7903(4) 0.7640(2) 0.8163(2) 0.0502(8) Uani 1 1 d . U . . .
S1 S 0.75348(11) 0.78867(8) 0.89367(7) 0.0355(2) Uani 1 1 d . 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
C1 C2 1.501(6) . ?
C1 N2 1.503(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.477(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.480(5) . ?
C3 C4 1.493(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.511(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.506(5) . ?
C5 C6 1.511(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.504(6) . ?
C7 C8 1.517(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.504(5) . ?
C9 C10 1.519(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.493(6) . ?
C11 C12 1.509(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N2 Pt1 2.079(3) . ?
N3 Pt1 2.004(3) . ?
N3 H3 0.9800 . ?
N4 Pt1 2.068(3) . ?
Pt1 O1A 2.044(3) . ?
Pt1 N1 2.044(3) . ?
N1 O1 1.163(8) . ?
N1 O2 1.217(9) . ?
N1A O2A 1.222(6) . ?
N1A O1A 1.320(5) . ?
C13 F3 1.330(5) . ?
C13 F1 1.333(5) . ?
C13 F2 1.335(5) . ?
C13 S1 1.808(4) . ?
O3 S1 1.430(3) . ?
O4 S1 1.444(3) . ?
O5 S1 1.433(3) . ?

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 N2 110.6(3) . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.4(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.7(4) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C3 C4 N4 109.9(3) . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
N4 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 116.9(4) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 114.1(4) . . ?
N2 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 116.8(4) . . ?
N4 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N4 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 114.1(4) . . ?
N4 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
N4 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1 N2 C7 110.1(3) . . ?
C1 N2 C5 110.2(4) . . ?
C7 N2 C5 109.4(3) . . ?
C1 N2 Pt1 105.8(2) . . ?
C7 N2 Pt1 115.6(3) . . ?
C5 N2 Pt1 105.6(2) . . ?
C2 N3 C3 116.9(3) . . ?
C2 N3 Pt1 107.7(2) . . ?
C3 N3 Pt1 107.3(2) . . ?
C2 N3 H3 108.2 . . ?
C3 N3 H3 108.2 . . ?
Pt1 N3 H3 108.2 . . ?
C11 N4 C9 108.8(3) . . ?
C11 N4 C4 110.3(3) . . ?
C9 N4 C4 109.6(4) . . ?
C11 N4 Pt1 116.0(3) . . ?
C9 N4 Pt1 106.5(2) . . ?
C4 N4 Pt1 105.5(2) . . ?
N3 Pt1 O1A 174.28(13) . . ?
N3 Pt1 N1 174.28(13) . . ?
N3 Pt1 N4 85.50(13) . . ?
O1A Pt1 N4 93.80(12) . . ?
N1 Pt1 N4 93.80(12) . . ?
N3 Pt1 N2 85.09(13) . . ?
O1A Pt1 N2 94.78(12) . . ?
N1 Pt1 N2 94.78(12) . . ?
N4 Pt1 N2 167.74(14) . . ?
O1 N1 O2 124.6(11) . . ?
O1 N1 Pt1 120.6(7) . . ?
O2 N1 Pt1 114.5(10) . . ?
O2A N1A O1A 111.9(5) . . ?
N1A O1A Pt1 125.9(3) . . ?
F3 C13 F1 107.3(3) . . ?
F3 C13 F2 107.2(3) . . ?
F1 C13 F2 106.9(3) . . ?
F3 C13 S1 111.8(3) . . ?
F1 C13 S1 111.5(3) . . ?
F2 C13 S1 111.9(3) . . ?
O3 S1 O5 116.2(2) . . ?
O3 S1 O4 114.9(2) . . ?
O5 S1 O4 114.2(2) . . ?
O3 S1 C13 103.2(2) . . ?
O5 S1 C13 103.2(2) . . ?
O4 S1 C13 102.5(2) . . ?

_refine_diff_density_max         1.028
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.113

####################################################################### 
# 
# 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_Pt_VT_250K
_database_code_depnum_ccdc_archive 'CCDC 1564480'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.2899(3)
_cell_length_b                   13.1228(4)
_cell_length_c                   17.2055(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.120(3)
_cell_angle_gamma                90
_cell_volume                     2085.56(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9100
_cell_measurement_theta_min      3.7900
_cell_measurement_theta_max      29.5770

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -5 0.1067
5 0 -4 0.0512
-1 5 1 0.2318
1 1 5 0.1103
1 -5 3 0.2517
1 0 5 0.1033
-5 0 4 0.0348
0 -1 -1 0.1437
5 1 -4 0.0508
3 -5 -2 0.1832
3 5 -2 0.1520
0 3 5 0.1696
_exptl_absorpt_coefficient_mu    6.884
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            22785
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.325
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4268
_reflns_number_gt                3705
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0216P)²+1.6373P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4268
_refine_ls_number_parameters     248
_refine_ls_number_restraints     213
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0516
_refine_ls_wR_factor_gt          0.0486
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

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 -0.0392(5) 0.5544(3) 0.8042(3) 0.0420(9) Uani 1 1 d . U . . .
H1A H -0.1313 0.5459 0.8251 0.050 Uiso 1 1 calc R U . . .
H1B H 0.0105 0.6118 0.8306 0.050 Uiso 1 1 calc R U . . .
C2 C -0.0651(4) 0.5760(3) 0.7182(2) 0.0394(8) Uani 1 1 d . U . . .
H2A H -0.1243 0.5230 0.6917 0.047 Uiso 1 1 calc R U . . .
H2B H -0.1137 0.6410 0.7089 0.047 Uiso 1 1 calc R U . . .
C3 C 0.0859(4) 0.5835(3) 0.6049(2) 0.0369(8) Uani 1 1 d . U . . .
H3A H 0.0566 0.6504 0.5851 0.044 Uiso 1 1 calc R U . . .
H3B H 0.0228 0.5328 0.5783 0.044 Uiso 1 1 calc R U . . .
C4 C 0.2412(4) 0.5629(3) 0.5929(2) 0.0402(8) Uani 1 1 d . U . . .
H4A H 0.3020 0.6174 0.6159 0.048 Uiso 1 1 calc R U . . .
H4B H 0.2513 0.5607 0.5374 0.048 Uiso 1 1 calc R U . . .
C5 C -0.0451(5) 0.3665(3) 0.8081(3) 0.0491(10) Uani 1 1 d . U . . .
H5A H 0.0163 0.3066 0.8113 0.059 Uiso 1 1 calc R U . . .
H5B H -0.0949 0.3689 0.7556 0.059 Uiso 1 1 calc R U . . .
C6 C -0.1579(6) 0.3530(4) 0.8652(3) 0.0819(18) Uani 1 1 d . U . . .
H6A H -0.2151 0.2936 0.8511 0.123 Uiso 1 1 calc R U . . .
H6B H -0.2195 0.4119 0.8632 0.123 Uiso 1 1 calc R U . . .
H6C H -0.1103 0.3450 0.9171 0.123 Uiso 1 1 calc R U . . .
C7 C 0.1242(5) 0.4616(3) 0.9016(3) 0.0505(10) Uani 1 1 d . U . . .
H7A H 0.1625 0.3943 0.9150 0.061 Uiso 1 1 calc R U . . .
H7B H 0.0530 0.4776 0.9371 0.061 Uiso 1 1 calc R U . . .
C8 C 0.2463(6) 0.5383(4) 0.9135(3) 0.0666(14) Uani 1 1 d . U . . .
H8A H 0.3170 0.5235 0.8783 0.100 Uiso 1 1 calc R U . . .
H8B H 0.2907 0.5344 0.9664 0.100 Uiso 1 1 calc R U . . .
H8C H 0.2085 0.6056 0.9034 0.100 Uiso 1 1 calc R U . . .
C9 C 0.2309(4) 0.3758(3) 0.5780(2) 0.0417(9) Uani 1 1 d . U . . .
H9A H 0.1263 0.3816 0.5699 0.050 Uiso 1 1 calc R U . . .
H9B H 0.2534 0.3123 0.6056 0.050 Uiso 1 1 calc R U . . .
C10 C 0.2874(5) 0.3691(4) 0.4987(3) 0.0592(12) Uani 1 1 d . U . . .
H10A H 0.2682 0.4319 0.4710 0.089 Uiso 1 1 calc R U . . .
H10B H 0.2399 0.3141 0.4693 0.089 Uiso 1 1 calc R U . . .
H10C H 0.3899 0.3568 0.5055 0.089 Uiso 1 1 calc R U . . .
C11 C 0.4517(4) 0.4579(3) 0.6416(3) 0.0494(10) Uani 1 1 d . U . . .
H11A H 0.4808 0.3885 0.6547 0.059 Uiso 1 1 calc R U . . .
H11B H 0.4889 0.4749 0.5926 0.059 Uiso 1 1 calc R U . . .
C12 C 0.5195(5) 0.5280(4) 0.7043(3) 0.0720(15) Uani 1 1 d . U . . .
H12A H 0.4968 0.5973 0.6902 0.108 Uiso 1 1 calc R U . . .
H12B H 0.6227 0.5189 0.7099 0.108 Uiso 1 1 calc R U . . .
H12C H 0.4825 0.5124 0.7529 0.108 Uiso 1 1 calc R U . . .
N2 N 0.0507(4) 0.4593(2) 0.81953(18) 0.0351(6) Uani 1 1 d . U . . .
N3 N 0.0796(3) 0.5783(2) 0.69014(17) 0.0275(6) Uani 1 1 d . U . . .
H3 H 0.1306 0.6381 0.7134 0.033 Uiso 1 1 calc R U . . .
N4 N 0.2890(3) 0.4628(2) 0.63003(18) 0.0328(6) Uani 1 1 d . U . . .
Pt1 Pt 0.18818(2) 0.45444(2) 0.73179(2) 0.02624(5) Uani 1 1 d . U . . .
N1 N 0.2939(4) 0.3289(3) 0.7722(2) 0.0425(8) Uani 1 1 d . U . . .
O1 O 0.2683(5) 0.2479(3) 0.7427(3) 0.0975(16) Uani 1 1 d . U . . .
O2 O 0.3924(6) 0.3305(3) 0.8243(3) 0.121(2) Uani 1 1 d . U . . .
C13 C 0.6113(5) 0.6888(3) 0.9128(3) 0.0471(8) Uani 1 1 d . U . . .
F1 F 0.6584(3) 0.59381(19) 0.91054(18) 0.0698(8) Uani 1 1 d . U . . .
F2 F 0.5561(3) 0.7000(2) 0.98043(18) 0.0759(8) Uani 1 1 d . U . . .
F3 F 0.5025(3) 0.6986(2) 0.85731(19) 0.0766(8) Uani 1 1 d . U . . .
O3 O 0.8570(4) 0.7599(3) 0.9667(2) 0.0745(10) Uani 1 1 d . U . . .
O4 O 0.6783(3) 0.8765(2) 0.90584(18) 0.0537(7) Uani 1 1 d . U . . .
O5 O 0.7944(4) 0.7571(2) 0.8262(2) 0.0637(8) Uani 1 1 d . U . . .
S1 S 0.75249(11) 0.78075(8) 0.90172(7) 0.0435(2) Uani 1 1 d . 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
C1 C2 1.500(6) . ?
C1 N2 1.510(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.476(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.475(5) . ?
C3 C4 1.503(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.507(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.509(5) . ?
C5 C6 1.521(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.502(5) . ?
C7 C8 1.513(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.514(5) . ?
C9 C10 1.516(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.504(6) . ?
C11 N4 1.505(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N2 Pt1 2.080(3) . ?
N3 Pt1 2.005(3) . ?
N3 H3 0.9800 . ?
N4 Pt1 2.075(3) . ?
Pt1 N1 2.004(3) . ?
N1 O1 1.190(5) . ?
N1 O2 1.211(4) . ?
C13 F3 1.321(5) . ?
C13 F1 1.322(5) . ?
C13 F2 1.329(5) . ?
C13 S1 1.807(4) . ?
O3 S1 1.427(3) . ?
O4 S1 1.438(3) . ?
O5 S1 1.430(3) . ?

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 N2 110.9(3) . . ?
C2 C1 H1A 109.5 . . ?
N2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 105.7(3) . . ?
N3 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N3 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.6(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
C3 C4 N4 110.0(3) . . ?
C3 C4 H4A 109.7 . . ?
N4 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
N4 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 116.6(4) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 113.6(4) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 116.1(4) . . ?
N4 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N4 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 114.0(4) . . ?
C12 C11 H11A 108.8 . . ?
N4 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
N4 C11 H11B 108.8 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 N2 C5 110.0(3) . . ?
C7 N2 C1 109.6(3) . . ?
C5 N2 C1 109.7(3) . . ?
C7 N2 Pt1 115.5(3) . . ?
C5 N2 Pt1 106.3(2) . . ?
C1 N2 Pt1 105.6(2) . . ?
C3 N3 C2 117.4(3) . . ?
C3 N3 Pt1 108.7(2) . . ?
C2 N3 Pt1 107.9(2) . . ?
C3 N3 H3 107.5 . . ?
C2 N3 H3 107.5 . . ?
Pt1 N3 H3 107.5 . . ?
C11 N4 C4 109.9(3) . . ?
C11 N4 C9 109.6(3) . . ?
C4 N4 C9 109.6(3) . . ?
C11 N4 Pt1 115.1(3) . . ?
C4 N4 Pt1 105.4(2) . . ?
C9 N4 Pt1 107.1(2) . . ?
N1 Pt1 N3 178.89(13) . . ?
N1 Pt1 N4 95.00(13) . . ?
N3 Pt1 N4 84.88(12) . . ?
N1 Pt1 N2 95.14(13) . . ?
N3 Pt1 N2 84.85(12) . . ?
N4 Pt1 N2 168.06(12) . . ?
O1 N1 O2 115.5(4) . . ?
O1 N1 Pt1 121.2(3) . . ?
O2 N1 Pt1 123.1(3) . . ?
F3 C13 F1 107.5(4) . . ?
F3 C13 F2 106.6(4) . . ?
F1 C13 F2 106.9(4) . . ?
F3 C13 S1 111.5(3) . . ?
F1 C13 S1 112.4(3) . . ?
F2 C13 S1 111.8(3) . . ?
O3 S1 O5 116.2(2) . . ?
O3 S1 O4 114.7(2) . . ?
O5 S1 O4 114.38(19) . . ?
O3 S1 C13 103.3(2) . . ?
O5 S1 C13 102.8(2) . . ?
O4 S1 C13 102.8(2) . . ?

_refine_diff_density_max         1.013
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_Pt_VT_300K
_database_code_depnum_ccdc_archive 'CCDC 1564477'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3533(5)
_cell_length_b                   13.1046(4)
_cell_length_c                   17.4169(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.472(4)
_cell_angle_gamma                90
_cell_volume                     2125.08(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    3100
_cell_measurement_theta_min      3.8790
_cell_measurement_theta_max      29.9930

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -5 0.1067
5 0 -4 0.0512
-1 5 1 0.2318
1 1 5 0.1103
1 -5 3 0.2517
1 0 5 0.1033
-5 0 4 0.0348
0 -1 -1 0.1437
5 1 -4 0.0508
3 -5 -2 0.1832
3 5 -2 0.1520
0 3 5 0.1696
_exptl_absorpt_coefficient_mu    6.756
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            11368
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.324
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4320
_reflns_number_gt                3353
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0351P)²+0.9292P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4320
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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 -0.0416(8) 0.5533(4) 0.8030(4) 0.0625(19) Uani 1 1 d . . . . .
H1A H -0.1337 0.5439 0.8232 0.075 Uiso 1 1 calc R U . . .
H1B H 0.0059 0.6109 0.8294 0.075 Uiso 1 1 calc R U . . .
C2 C -0.0650(7) 0.5757(5) 0.7180(4) 0.0582(18) Uani 1 1 d . . . . .
H2A H -0.1237 0.5230 0.6916 0.070 Uiso 1 1 calc R U . . .
H2B H -0.1127 0.6409 0.7092 0.070 Uiso 1 1 calc R U . . .
C3 C 0.0858(8) 0.5818(5) 0.6059(4) 0.0553(17) Uani 1 1 d . . . . .
H3A H 0.0557 0.6482 0.5857 0.066 Uiso 1 1 calc R U . . .
H3B H 0.0245 0.5300 0.5802 0.066 Uiso 1 1 calc R U . . .
C4 C 0.2407(8) 0.5623(4) 0.5940(4) 0.0587(18) Uani 1 1 d . . . . .
H4A H 0.2519 0.5604 0.5393 0.070 Uiso 1 1 calc R U . . .
H4B H 0.2997 0.6173 0.6169 0.070 Uiso 1 1 calc R U . . .
C5 C -0.0473(9) 0.3642(5) 0.8070(4) 0.072(2) Uani 1 1 d . . . . .
H5A H -0.0952 0.3666 0.7551 0.086 Uiso 1 1 calc R U . . .
H5B H 0.0133 0.3040 0.8103 0.086 Uiso 1 1 calc R U . . .
C6 C -0.1602(12) 0.3514(7) 0.8626(6) 0.116(4) Uani 1 1 d . . . . .
H6A H -0.2198 0.2939 0.8474 0.174 Uiso 1 1 calc R U . . .
H6B H -0.2183 0.4119 0.8622 0.174 Uiso 1 1 calc R U . . .
H6C H -0.1145 0.3404 0.9136 0.174 Uiso 1 1 calc R U . . .
C7 C 0.1193(10) 0.4602(5) 0.8992(4) 0.074(2) Uani 1 1 d . . . . .
H7A H 0.1585 0.3931 0.9120 0.089 Uiso 1 1 calc R U . . .
H7B H 0.0470 0.4747 0.9341 0.089 Uiso 1 1 calc R U . . .
C8 C 0.2379(11) 0.5380(6) 0.9118(5) 0.092(3) Uani 1 1 d . . . . .
H8A H 0.3052 0.5284 0.8742 0.138 Uiso 1 1 calc R U . . .
H8B H 0.2861 0.5298 0.9626 0.138 Uiso 1 1 calc R U . . .
H8C H 0.1978 0.6054 0.9067 0.138 Uiso 1 1 calc R U . . .
C9 C 0.2324(8) 0.3744(5) 0.5791(4) 0.0601(18) Uani 1 1 d . . . . .
H9A H 0.2556 0.3111 0.6063 0.072 Uiso 1 1 calc R U . . .
H9B H 0.1285 0.3795 0.5715 0.072 Uiso 1 1 calc R U . . .
C10 C 0.2898(9) 0.3686(6) 0.5003(4) 0.083(2) Uani 1 1 d . . . . .
H10A H 0.2666 0.4305 0.4723 0.124 Uiso 1 1 calc R U . . .
H10B H 0.2468 0.3117 0.4721 0.124 Uiso 1 1 calc R U . . .
H10C H 0.3922 0.3600 0.5068 0.124 Uiso 1 1 calc R U . . .
C11 C 0.4498(8) 0.4582(5) 0.6412(5) 0.068(2) Uani 1 1 d . . . . .
H11A H 0.4873 0.4754 0.5927 0.082 Uiso 1 1 calc R U . . .
H11B H 0.4788 0.3888 0.6541 0.082 Uiso 1 1 calc R U . . .
C12 C 0.5160(10) 0.5287(7) 0.7031(6) 0.103(3) Uani 1 1 d . . . . .
H12A H 0.5093 0.5978 0.6850 0.155 Uiso 1 1 calc R U . . .
H12B H 0.6152 0.5110 0.7154 0.155 Uiso 1 1 calc R U . . .
H12C H 0.4658 0.5220 0.7484 0.155 Uiso 1 1 calc R U . . .
N2 N 0.0493(6) 0.4581(3) 0.8186(3) 0.0493(13) Uani 1 1 d . . . . .
N3 N 0.0787(5) 0.5778(3) 0.6901(3) 0.0403(11) Uani 1 1 d . . . . .
H3 H 0.1290 0.6380 0.7126 0.048 Uiso 1 1 calc R U . . .
N4 N 0.2890(5) 0.4628(3) 0.6303(3) 0.0430(11) Uani 1 1 d . . . . .
Pt1 Pt 0.18682(2) 0.45368(2) 0.73119(2) 0.03743(9) Uani 1 1 d . . . . .
N1 N 0.2934(7) 0.3279(4) 0.7704(3) 0.0594(15) Uani 1 1 d . . . . .
O1 O 0.2665(10) 0.2474(5) 0.7427(4) 0.141(2) Uani 1 1 d . . . . .
O2 O 0.3886(9) 0.3289(4) 0.8212(4) 0.141(2) Uani 1 1 d . . . . .
C13 C 0.6117(9) 0.6876(5) 0.9151(5) 0.0651(19) Uani 1 1 d . . . . .
F1 F 0.6605(6) 0.5930(3) 0.9126(3) 0.1016(17) Uani 1 1 d . . . . .
F2 F 0.5575(6) 0.6992(4) 0.9814(3) 0.1104(18) Uani 1 1 d . . . . .
F3 F 0.5057(6) 0.6972(4) 0.8599(3) 0.1087(18) Uani 1 1 d . . . . .
O3 O 0.8537(6) 0.7598(4) 0.9665(4) 0.105(2) Uani 1 1 d . . . . .
O4 O 0.6778(6) 0.8752(3) 0.9074(3) 0.0751(15) Uani 1 1 d . . . . .
O5 O 0.7925(7) 0.7564(4) 0.8280(3) 0.0924(19) Uani 1 1 d . . . . .
S1 S 0.7510(2) 0.78048(12) 0.90296(11) 0.0608(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.503(10) . ?
C1 N2 1.519(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.472(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.476(8) . ?
C3 C4 1.504(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.500(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.509(10) . ?
C5 N2 1.528(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N2 1.491(9) . ?
C7 C8 1.507(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.523(9) . ?
C9 N4 1.526(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.499(8) . ?
C11 C12 1.508(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N2 Pt1 2.086(5) . ?
N3 Pt1 2.011(4) . ?
N3 H3 0.9800 . ?
N4 Pt1 2.082(5) . ?
Pt1 N1 2.012(5) . ?
N1 O1 1.177(8) . ?
N1 O2 1.193(7) . ?
C13 F2 1.314(8) . ?
C13 F3 1.320(8) . ?
C13 F1 1.323(8) . ?
C13 S1 1.811(8) . ?
O3 S1 1.420(6) . ?
O4 S1 1.424(4) . ?
O5 S1 1.433(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N2 111.3(5) . . ?
C2 C1 H1A 109.4 . . ?
N2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N3 C2 C1 106.0(6) . . ?
N3 C2 H2A 110.5 . . ?
C1 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C3 C4 105.4(5) . . ?
N3 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
N3 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
N4 C4 C3 110.2(5) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 N2 116.4(6) . . ?
C6 C5 H5A 108.2 . . ?
N2 C5 H5A 108.2 . . ?
C6 C5 H5B 108.2 . . ?
N2 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 113.6(6) . . ?
N2 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N2 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N4 115.6(6) . . ?
C10 C9 H9A 108.4 . . ?
N4 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
N4 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 113.8(6) . . ?
N4 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N4 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 N2 C1 110.0(5) . . ?
C7 N2 C5 109.9(5) . . ?
C1 N2 C5 108.9(6) . . ?
C7 N2 Pt1 116.2(5) . . ?
C1 N2 Pt1 105.3(4) . . ?
C5 N2 Pt1 106.2(4) . . ?
C2 N3 C3 117.2(5) . . ?
C2 N3 Pt1 108.1(3) . . ?
C3 N3 Pt1 108.2(3) . . ?
C2 N3 H3 107.6 . . ?
C3 N3 H3 107.6 . . ?
Pt1 N3 H3 107.6 . . ?
C11 N4 C4 110.3(5) . . ?
C11 N4 C9 109.4(5) . . ?
C4 N4 C9 109.9(5) . . ?
C11 N4 Pt1 115.3(4) . . ?
C4 N4 Pt1 105.1(4) . . ?
C9 N4 Pt1 106.7(4) . . ?
N3 Pt1 N1 178.9(2) . . ?
N3 Pt1 N4 84.79(19) . . ?
N1 Pt1 N4 94.6(2) . . ?
N3 Pt1 N2 85.01(19) . . ?
N1 Pt1 N2 95.4(2) . . ?
N4 Pt1 N2 168.30(19) . . ?
O1 N1 O2 115.4(6) . . ?
O1 N1 Pt1 121.0(5) . . ?
O2 N1 Pt1 123.6(5) . . ?
F2 C13 F3 107.7(7) . . ?
F2 C13 F1 107.6(6) . . ?
F3 C13 F1 107.6(6) . . ?
F2 C13 S1 111.5(5) . . ?
F3 C13 S1 110.4(5) . . ?
F1 C13 S1 111.8(6) . . ?
O3 S1 O4 114.6(4) . . ?
O3 S1 O5 116.5(4) . . ?
O4 S1 O5 114.5(3) . . ?
O3 S1 C13 102.8(4) . . ?
O4 S1 C13 103.0(3) . . ?
O5 S1 C13 102.7(4) . . ?

_refine_diff_density_max         1.100
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_Pt_VT_210K
_database_code_depnum_ccdc_archive 'CCDC 1564478'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2017-09-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
"Nitro(N,N,N',N'-tetraethyldiethylenetriamine)platinum(II) trifluoromethanesulfonate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H29 N4 O2 Pt, C1 F3 O3 S'
_chemical_formula_sum            'C13 H29 F3 N4 O5 Pt S'
_chemical_formula_weight         605.55

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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   9.3316(2)
_cell_length_b                   12.9806(3)
_cell_length_c                   16.7653(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.125(2)
_cell_angle_gamma                90
_cell_volume                     2005.08(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    9810
_cell_measurement_theta_min      3.8150
_cell_measurement_theta_max      29.6020

_exptl_crystal_description       shard
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.485
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.086
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 5 0.1067
0 3 -5 0.1696
-3 5 2 0.1520
-3 -5 2 0.1832
-5 1 4 0.0508
0 -1 1 0.1437
-1 0 -5 0.1033
-1 -5 -3 0.2517
-1 1 -5 0.1103
1 5 -1 0.2318
-5 0 4 0.0512
5 0 -4 0.0348
_exptl_absorpt_coefficient_mu    7.161
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            21932
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.372
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4094
_reflns_number_gt                3645
_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'

_refine_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)+(0.0183P)²+0.6545P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4094
_refine_ls_number_parameters     255
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0191
_refine_ls_wR_factor_ref         0.0429
_refine_ls_wR_factor_gt          0.0410
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.002
_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 -0.0075(4) 0.5637(2) 0.8170(2) 0.0307(7) Uani 1 1 d . U . . .
H1A H -0.0977 0.5545 0.8392 0.037 Uiso 1 1 calc R U . . .
H1B H 0.0447 0.6226 0.8443 0.037 Uiso 1 1 calc R U . . .
C2 C -0.0425(3) 0.5846(2) 0.72795(19) 0.0308(7) Uani 1 1 d . U . . .
H2A H -0.1046 0.5300 0.7008 0.037 Uiso 1 1 calc R U . . .
H2B H -0.0933 0.6506 0.7181 0.037 Uiso 1 1 calc R U . . .
C3 C 0.0899(4) 0.5847(2) 0.60830(19) 0.0319(7) Uani 1 1 d . U . . .
H3A H 0.0542 0.6505 0.5843 0.038 Uiso 1 1 calc R U . . .
H3B H 0.0242 0.5298 0.5850 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2420(4) 0.5643(2) 0.5927(2) 0.0327(7) Uani 1 1 d . U . . .
H4A H 0.2421 0.5577 0.5345 0.039 Uiso 1 1 calc R U . . .
H4B H 0.3051 0.6222 0.6127 0.039 Uiso 1 1 calc R U . . .
C5 C -0.0093(3) 0.3728(2) 0.81914(19) 0.0307(7) Uani 1 1 d . U . . .
H5A H 0.0544 0.3124 0.8223 0.037 Uiso 1 1 calc R U . . .
H5B H -0.0638 0.3754 0.7642 0.037 Uiso 1 1 calc R U . . .
C6 C -0.1171(4) 0.3568(3) 0.8777(2) 0.0448(9) Uani 1 1 d . U . . .
H6A H -0.1750 0.2958 0.8620 0.067 Uiso 1 1 calc R U . . .
H6B H -0.1802 0.4163 0.8762 0.067 Uiso 1 1 calc R U . . .
H6C H -0.0646 0.3479 0.9320 0.067 Uiso 1 1 calc R U . . .
C7 C 0.1657(4) 0.4684(2) 0.91727(19) 0.0314(7) Uani 1 1 d . U . . .
H7A H 0.2132 0.4014 0.9284 0.038 Uiso 1 1 calc R U . . .
H7B H 0.0956 0.4766 0.9546 0.038 Uiso 1 1 calc R U . . .
C8 C 0.2789(4) 0.5522(3) 0.9341(2) 0.0400(8) Uani 1 1 d . U . . .
H8A H 0.3395 0.5520 0.8921 0.060 Uiso 1 1 calc R U . . .
H8B H 0.3386 0.5398 0.9860 0.060 Uiso 1 1 calc R U . . .
H8C H 0.2313 0.6185 0.9349 0.060 Uiso 1 1 calc R U . . .
C9 C 0.2370(3) 0.3745(2) 0.58711(19) 0.0311(7) Uani 1 1 d . U . . .
H9A H 0.1309 0.3786 0.5801 0.037 Uiso 1 1 calc R U . . .
H9B H 0.2661 0.3128 0.6193 0.037 Uiso 1 1 calc R U . . .
C10 C 0.2809(4) 0.3599(3) 0.5043(2) 0.0391(8) Uani 1 1 d . U . . .
H10A H 0.2564 0.4213 0.4720 0.059 Uiso 1 1 calc R U . . .
H10B H 0.2296 0.3012 0.4776 0.059 Uiso 1 1 calc R U . . .
H10C H 0.3847 0.3479 0.5103 0.059 Uiso 1 1 calc R U . . .
C11 C 0.4618(3) 0.4637(2) 0.6439(2) 0.0338(7) Uani 1 1 d . U . . .
H11A H 0.4956 0.3966 0.6663 0.041 Uiso 1 1 calc R U . . .
H11B H 0.4903 0.4696 0.5903 0.041 Uiso 1 1 calc R U . . .
C12 C 0.5362(4) 0.5471(3) 0.6972(3) 0.0519(10) Uani 1 1 d . U . . .
H12A H 0.5300 0.6116 0.6677 0.078 Uiso 1 1 calc R U . . .
H12B H 0.6374 0.5289 0.7139 0.078 Uiso 1 1 calc R U . . .
H12C H 0.4893 0.5546 0.7446 0.078 Uiso 1 1 calc R U . . .
N2 N 0.0848(3) 0.46777(17) 0.83222(16) 0.0249(5) Uani 1 1 d . U . . .
N3 N 0.0984(3) 0.58765(18) 0.69742(14) 0.0247(5) Uani 1 1 d . U . . .
H3 H 0.1517 0.6505 0.7184 0.030 Uiso 1 1 calc R U . . .
N4 N 0.2982(3) 0.46690(17) 0.63480(16) 0.0248(5) Uani 1 1 d . U . . .
Pt1 Pt 0.21254(2) 0.46376(2) 0.74156(2) 0.02013(5) Uani 1 1 d . U . . .
N1 N 0.3128(2) 0.32810(16) 0.77936(13) 0.0310(5) Uani 0.079(4) 1 d D U P A 1
O1 O 0.276(2) 0.2487(12) 0.7486(13) 0.0310(5) Uani 0.079(4) 1 d D U P A 1
O2 O 0.408(3) 0.337(2) 0.8360(15) 0.0310(5) Uani 0.079(4) 1 d D U P A 1
N1A N 0.4394(4) 0.3229(3) 0.8278(2) 0.0439(10) Uani 0.921(4) 1 d D U P A 2
O1A O 0.3128(2) 0.32810(16) 0.77936(13) 0.0310(5) Uani 0.921(4) 1 d D U P A 2
O2A O 0.4895(3) 0.4055(2) 0.84931(19) 0.0581(9) Uani 0.921(4) 1 d D U P A 2
C13 C 0.6087(3) 0.7001(2) 0.9026(2) 0.0300(6) Uani 1 1 d . U . . .
F1 F 0.6528(2) 0.60276(14) 0.89948(12) 0.0435(5) Uani 1 1 d . U . . .
F2 F 0.5603(2) 0.71150(15) 0.97303(12) 0.0482(5) Uani 1 1 d . U . . .
F3 F 0.49510(19) 0.71255(14) 0.84454(12) 0.0416(5) Uani 1 1 d . U . . .
O3 O 0.8602(3) 0.76673(19) 0.96066(16) 0.0490(6) Uani 1 1 d . U . . .
O4 O 0.6823(3) 0.88877(16) 0.89583(14) 0.0388(5) Uani 1 1 d . U . . .
O5 O 0.7893(3) 0.76494(18) 0.81502(15) 0.0438(6) Uani 1 1 d . U . . .
S1 S 0.75245(8) 0.78999(6) 0.89241(5) 0.02979(17) Uani 1 1 d . 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
C1 C2 1.502(4) . ?
C1 N2 1.512(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.486(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.484(4) . ?
C3 C4 1.506(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.502(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.509(4) . ?
C5 C6 1.527(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N2 1.504(4) . ?
C7 C8 1.512(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N4 1.503(4) . ?
C9 C10 1.521(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 C12 1.502(5) . ?
C11 N4 1.511(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
N2 Pt1 2.076(3) . ?
N3 Pt1 2.004(2) . ?
N3 H3 0.9900 . ?
N4 Pt1 2.073(3) . ?
Pt1 O1A 2.047(2) . ?
Pt1 N1 2.047(2) . ?
N1 O1 1.179(9) . ?
N1 O2 1.201(10) . ?
N1A O2A 1.202(4) . ?
N1A O1A 1.325(4) . ?
C13 F3 1.331(4) . ?
C13 F1 1.332(4) . ?
C13 F2 1.337(4) . ?
C13 S1 1.806(3) . ?
O3 S1 1.431(2) . ?
O4 S1 1.445(2) . ?
O5 S1 1.431(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 N2 110.2(2) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.4(2) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.1(3) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 109.6(3) . . ?
N4 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N4 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C6 116.5(3) . . ?
N2 C5 H5A 108.2 . . ?
C6 C5 H5A 108.2 . . ?
N2 C5 H5B 108.2 . . ?
C6 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 C8 114.3(3) . . ?
N2 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N2 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 116.8(3) . . ?
N4 C9 H9A 108.1 . . ?
C10 C9 H9A 108.1 . . ?
N4 C9 H9B 108.1 . . ?
C10 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N4 113.8(3) . . ?
C12 C11 H11A 108.8 . . ?
N4 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
N4 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 N2 C5 109.6(2) . . ?
C7 N2 C1 110.0(2) . . ?
C5 N2 C1 110.2(3) . . ?
C7 N2 Pt1 115.7(2) . . ?
C5 N2 Pt1 105.16(17) . . ?
C1 N2 Pt1 105.96(18) . . ?
C3 N3 C2 115.9(2) . . ?
C3 N3 Pt1 106.94(17) . . ?
C2 N3 Pt1 107.41(17) . . ?
C3 N3 H3 108.8 . . ?
C2 N3 H3 108.8 . . ?
Pt1 N3 H3 108.8 . . ?
C4 N4 C9 110.3(3) . . ?
C4 N4 C11 110.1(2) . . ?
C9 N4 C11 108.9(2) . . ?
C4 N4 Pt1 105.57(17) . . ?
C9 N4 Pt1 106.13(18) . . ?
C11 N4 Pt1 115.7(2) . . ?
N3 Pt1 O1A 173.98(9) . . ?
N3 Pt1 N1 173.98(9) . . ?
N3 Pt1 N4 85.44(9) . . ?
O1A Pt1 N4 93.69(9) . . ?
N1 Pt1 N4 93.69(9) . . ?
N3 Pt1 N2 85.24(9) . . ?
O1A Pt1 N2 94.72(9) . . ?
N1 Pt1 N2 94.72(9) . . ?
N4 Pt1 N2 167.55(10) . . ?
O1 N1 O2 124.3(14) . . ?
O1 N1 Pt1 121.9(11) . . ?
O2 N1 Pt1 113.8(14) . . ?
O2A N1A O1A 113.9(3) . . ?
N1A O1A Pt1 123.6(2) . . ?
F3 C13 F1 107.5(2) . . ?
F3 C13 F2 106.9(2) . . ?
F1 C13 F2 106.8(3) . . ?
F3 C13 S1 111.7(2) . . ?
F1 C13 S1 111.7(2) . . ?
F2 C13 S1 111.8(2) . . ?
O3 S1 O5 115.95(16) . . ?
O3 S1 O4 114.90(15) . . ?
O5 S1 O4 114.39(14) . . ?
O3 S1 C13 103.07(15) . . ?
O5 S1 C13 103.17(15) . . ?
O4 S1 C13 102.80(15) . . ?

_refine_diff_density_max         0.815
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.093

