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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_nrb143
_audit_creation_date             2014-05-05
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            
;
 tetrakis(N-methylimidazole) palladium(II) bistriflimide
;
_chemical_name_systematic        
;
 tetrakis(N-methylimidazole) palladium(II) bis(trifluoromethyl)sulfonyl imide
;
_chemical_formula_moiety         'C16 H24 N8 Pd, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C20 H24 F12 N10 O8 Pd S4'
_chemical_formula_weight         995.13
_chemical_melting_point          378
_chemical_oxdiff_formula         'Pd C3 H3 N2 C H4 C2 F6 S2 O4 N'
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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   9.1556(2)
_cell_length_b                   10.8229(2)
_cell_length_c                   17.9774(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.330(2)
_cell_angle_gamma                90.00
_cell_volume                     1757.82(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5107
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.860
_cell_measurement_theta_min      2.946
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8254
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         2.94
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0647870000
_diffrn_orient_matrix_UB_12      0.0204441000
_diffrn_orient_matrix_UB_13      0.0132745000
_diffrn_orient_matrix_UB_21      0.0099454000
_diffrn_orient_matrix_UB_22      -0.0466243000
_diffrn_orient_matrix_UB_23      0.0280654000
_diffrn_orient_matrix_UB_31      0.0432768000
_diffrn_orient_matrix_UB_32      0.0412522000
_diffrn_orient_matrix_UB_33      0.0251799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                3632
_reflns_number_total             4114
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0256
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0233P)²+1.1985P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0615
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C13')
Uanis(F14) = Uanis(F14')
Uanis(F15) = Uanis(F15')
Uanis(F16) = Uanis(F16')
Uanis(S17) = Uanis(S17')
Uanis(O18) = Uanis(O18')
Uanis(O19) = Uanis(O19')
Uanis(N20) = Uanis(N20')
Uanis(S21) = Uanis(S21')
Uanis(O22) = Uanis(O22')
Uanis(O23) = Uanis(O23')
Uanis(C24) = Uanis(C24')
Uanis(F25) = Uanis(F25')
Uanis(F26) = Uanis(F26')
Uanis(F27) = Uanis(F27')
3. Same fragment restrains
{C13, F14, F15, F16, S17, O18, O19, N20, S21, O22, O23, C24, F25, F26, F27}
as
{C13', F14', F15', F16', S17', O18', O19', N20', S21', O22', O23', C24', F25',
F26', F27'}
4. Others
 Sof(C13')=Sof(F14')=Sof(F15')=Sof(F16')=Sof(S17')=Sof(O18')=Sof(O19')=
 Sof(N20')=Sof(S21')=Sof(O22')=Sof(O23')=Sof(C24')=Sof(F25')=Sof(F26')=
 Sof(F27')=1-FVAR(1)
 Sof(C13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(S17)=Sof(O18)=Sof(O19)=Sof(N20)=
 Sof(S21)=Sof(O22)=Sof(O23)=Sof(C24)=Sof(F25)=Sof(F26)=Sof(F27)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 0.5000 0.5000 0.01348(6) Uani 1 d . . 2 S T P
N1 N 0.44033(17) 0.66453(14) 0.45231(9) 0.0154(3) Uani 1 d . . 1 . . .
C2 C 0.39716(19) 0.68247(17) 0.37907(11) 0.0156(4) Uani 1 d . . 1 . . .
H2 H 0.3920 0.6214 0.3424 0.019 Uiso 1 calc . . 1 R . .
N3 N 0.36198(17) 0.80160(15) 0.36564(9) 0.0164(3) Uani 1 d . . 1 . . .
C4 C 0.3850(2) 0.86294(18) 0.43329(11) 0.0208(4) Uani 1 d . . 1 . . .
H4 H 0.3700 0.9466 0.4410 0.025 Uiso 1 calc . . 1 R . .
C5 C 0.4335(2) 0.77785(18) 0.48641(11) 0.0205(4) Uani 1 d . . 1 . . .
H5 H 0.4584 0.7932 0.5378 0.025 Uiso 1 calc . . 1 R . .
C6 C 0.3090(2) 0.8557(2) 0.29169(11) 0.0239(4) Uani 1 d . . 1 . . .
H6A H 0.3787 0.9163 0.2803 0.036 Uiso 1 calc . . 1 GR . .
H6B H 0.2148 0.8944 0.2921 0.036 Uiso 1 calc . . 1 GR . .
H6C H 0.2986 0.7920 0.2541 0.036 Uiso 1 calc . . 1 GR . .
N7 N 0.68638(17) 0.50688(14) 0.45396(9) 0.0157(3) Uani 1 d . . 1 . . .
C8 C 0.7797(2) 0.60105(17) 0.45916(10) 0.0170(4) Uani 1 d . . 1 . . .
H8 H 0.7677 0.6746 0.4842 0.020 Uiso 1 calc . . 1 R . .
N9 N 0.89336(17) 0.57586(14) 0.42347(9) 0.0162(3) Uani 1 d . . 1 . . .
C10 C 0.8716(2) 0.46008(19) 0.39325(11) 0.0220(4) Uani 1 d . . 1 . . .
H10 H 0.9326 0.4187 0.3649 0.026 Uiso 1 calc . . 1 R . .
C11 C 0.7438(2) 0.4173(2) 0.41261(12) 0.0231(4) Uani 1 d . . 1 . . .
H11 H 0.7019 0.3403 0.4001 0.028 Uiso 1 calc . . 1 R . .
C12 C 1.0172(2) 0.65775(18) 0.41610(12) 0.0221(4) Uani 1 d . . 1 . . .
H12A H 1.0084 0.6859 0.3649 0.033 Uiso 1 calc . . 1 GR . .
H12B H 1.1087 0.6136 0.4295 0.033 Uiso 1 calc . . 1 GR . .
H12C H 1.0159 0.7275 0.4490 0.033 Uiso 1 calc . . 1 GR . .
C13 C 0.9027(3) 0.4311(2) 0.88393(13) 0.0244(5) Uani 0.9457(10) d A 1 1 . . .
F14 F 1.0236(2) 0.4940(2) 0.87743(15) 0.0362(4) Uani 0.9457(10) d A 1 1 . . .
F15 F 0.90047(18) 0.32767(14) 0.84443(9) 0.0431(4) Uani 0.9457(10) d A 1 1 . .
.
F16 F 0.90956(17) 0.40029(15) 0.95600(8) 0.0377(4) Uani 0.9457(10) d A 1 1 . .
.
S17 S 0.73411(7) 0.52195(5) 0.85404(3) 0.01622(13) Uani 0.9457(10) d A 1 1 . .
.
O18 O 0.76161(17) 0.63713(14) 0.89246(8) 0.0239(3) Uani 0.9457(10) d A 1 1 . .
.
O19 O 0.61907(19) 0.44380(17) 0.87200(9) 0.0271(4) Uani 0.9457(10) d A 1 1 . .
.
N20 N 0.71795(19) 0.52770(15) 0.76515(10) 0.0180(4) Uani 0.9457(10) d A 1 1 . .
.
S21 S 0.79823(7) 0.62454(5) 0.72036(3) 0.01657(12) Uani 0.9457(10) d A 1 1 . .
.
O22 O 0.93615(16) 0.67122(15) 0.75801(9) 0.0253(4) Uani 0.9457(10) d A 1 1 . .
.
O23 O 0.79044(19) 0.58027(15) 0.64487(9) 0.0286(4) Uani 0.9457(10) d A 1 1 . .
.
C24 C 0.6748(2) 0.7584(2) 0.70829(12) 0.0236(5) Uani 0.9457(10) d A 1 1 . . .
F25 F 0.6684(2) 0.81627(14) 0.77226(9) 0.0443(4) Uani 0.9457(10) d A 1 1 . . .
F26 F 0.53916(15) 0.72191(14) 0.67923(9) 0.0429(4) Uani 0.9457(10) d A 1 1 . .
.
F27 F 0.7190(3) 0.8371(2) 0.66019(9) 0.0331(4) Uani 0.9457(10) d A 1 1 . . .
C13' C 0.927(3) 0.441(2) 0.8738(14) 0.0244(5) Uani 0.0543(10) d A 2 1 . . .
F14' F 1.049(4) 0.506(4) 0.887(3) 0.0362(4) Uani 0.0543(10) d A 2 1 . . .
F15' F 0.931(3) 0.387(2) 0.8078(13) 0.0431(4) Uani 0.0543(10) d A 2 1 . . .
F16' F 0.935(3) 0.352(2) 0.9256(14) 0.0377(4) Uani 0.0543(10) d A 2 1 . . .
S17' S 0.7580(14) 0.5339(11) 0.8761(6) 0.01622(13) Uani 0.0543(10) d A 2 1 . .
.
O18' O 0.768(3) 0.575(2) 0.9513(10) 0.0239(3) Uani 0.0543(10) d A 2 1 . . .
O19' O 0.644(3) 0.446(3) 0.8490(17) 0.0271(4) Uani 0.0543(10) d A 2 1 . . .
N20' N 0.772(3) 0.6386(18) 0.8186(8) 0.0180(4) Uani 0.0543(10) d A 2 1 . . .
S21' S 0.7359(12) 0.6405(8) 0.7314(5) 0.01657(12) Uani 0.0543(10) d A 2 1 . . .
O22' O 0.593(2) 0.591(2) 0.6993(13) 0.0253(4) Uani 0.0543(10) d A 2 1 . . .
O23' O 0.852(3) 0.604(2) 0.6895(14) 0.0286(4) Uani 0.0543(10) d A 2 1 . . .
C24' C 0.721(2) 0.8086(15) 0.7158(14) 0.0236(5) Uani 0.0543(10) d A 2 1 . . .
F25' F 0.616(3) 0.854(2) 0.7505(16) 0.0443(4) Uani 0.0543(10) d A 2 1 . . .
F26' F 0.848(2) 0.862(2) 0.7469(15) 0.0429(4) Uani 0.0543(10) d A 2 1 . . .
F27' F 0.699(6) 0.838(4) 0.6447(15) 0.0331(4) Uani 0.0543(10) d A 2 1 . . .


_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
Pd1 N1 2.0131(15) 3_666 ?
Pd1 N1 2.0131(15) . ?
Pd1 N7 2.0151(16) . ?
Pd1 N7 2.0151(16) 3_666 ?
N1 C2 1.326(2) . ?
N1 C5 1.377(2) . ?
C2 N3 1.341(2) . ?
N3 C4 1.372(2) . ?
N3 C6 1.462(2) . ?
C4 C5 1.349(3) . ?
N7 C8 1.323(2) . ?
N7 C11 1.377(2) . ?
C8 N9 1.337(2) . ?
N9 C10 1.367(3) . ?
N9 C12 1.462(2) . ?
C10 C11 1.355(3) . ?
C13 F14 1.320(3) . ?
C13 F15 1.325(3) . ?
C13 F16 1.329(3) . ?
C13 S17 1.835(2) . ?
S17 O18 1.4277(16) . ?
S17 O19 1.4280(16) . ?
S17 N20 1.5820(18) . ?
N20 S21 1.5745(18) . ?
S21 O22 1.4250(15) . ?
S21 O23 1.4301(16) . ?
S21 C24 1.829(2) . ?
C24 F25 1.319(3) . ?
C24 F26 1.327(3) . ?
C24 F27 1.323(3) . ?
C13' F14' 1.313(18) . ?
C13' F15' 1.330(18) . ?
C13' F16' 1.329(18) . ?
C13' S17' 1.850(16) . ?
S17' O18' 1.411(15) . ?
S17' O19' 1.443(17) . ?
S17' N20' 1.554(15) . ?
N20' S21' 1.549(15) . ?
S21' O22' 1.442(15) . ?
S21' O23' 1.450(16) . ?
S21' C24' 1.842(16) . ?
C24' F25' 1.323(18) . ?
C24' F26' 1.335(18) . ?
C24' F27' 1.298(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 N1 180.0 3_666 . ?
N1 Pd1 N7 88.95(6) . . ?
N1 Pd1 N7 91.05(6) . 3_666 ?
N1 Pd1 N7 91.05(6) 3_666 . ?
N1 Pd1 N7 88.95(6) 3_666 3_666 ?
N7 Pd1 N7 179.998(1) . 3_666 ?
C2 N1 Pd1 124.68(13) . . ?
C2 N1 C5 106.49(16) . . ?
C5 N1 Pd1 128.82(13) . . ?
N1 C2 N3 110.10(17) . . ?
C2 N3 C4 107.93(16) . . ?
C2 N3 C6 125.70(17) . . ?
C4 N3 C6 126.38(17) . . ?
C5 C4 N3 106.43(17) . . ?
C4 C5 N1 109.05(17) . . ?
C8 N7 Pd1 125.40(13) . . ?
C8 N7 C11 106.39(16) . . ?
C11 N7 Pd1 128.21(13) . . ?
N7 C8 N9 110.67(17) . . ?
C8 N9 C10 107.62(16) . . ?
C8 N9 C12 126.57(17) . . ?
C10 N9 C12 125.79(17) . . ?
C11 C10 N9 106.72(18) . . ?
C10 C11 N7 108.59(18) . . ?
F14 C13 F15 109.2(2) . . ?
F14 C13 F16 107.9(2) . . ?
F14 C13 S17 112.06(17) . . ?
F15 C13 F16 107.71(19) . . ?
F15 C13 S17 110.91(16) . . ?
F16 C13 S17 108.95(17) . . ?
O18 S17 C13 104.59(10) . . ?
O18 S17 O19 119.11(11) . . ?
O18 S17 N20 115.76(9) . . ?
O19 S17 C13 103.46(11) . . ?
O19 S17 N20 107.46(10) . . ?
N20 S17 C13 104.68(11) . . ?
S21 N20 S17 124.60(11) . . ?
N20 S21 C24 104.90(10) . . ?
O22 S21 N20 116.38(9) . . ?
O22 S21 O23 118.27(11) . . ?
O22 S21 C24 104.99(10) . . ?
O23 S21 N20 107.86(10) . . ?
O23 S21 C24 102.59(10) . . ?
F25 C24 S21 112.73(15) . . ?
F25 C24 F26 108.3(2) . . ?
F25 C24 F27 109.0(2) . . ?
F26 C24 S21 109.37(16) . . ?
F27 C24 S21 109.78(18) . . ?
F27 C24 F26 107.49(19) . . ?
F14' C13' F15' 105(3) . . ?
F14' C13' F16' 108(3) . . ?
F14' C13' S17' 113(2) . . ?
F15' C13' S17' 114.0(17) . . ?
F16' C13' F15' 108(2) . . ?
F16' C13' S17' 109.2(18) . . ?
O18' S17' C13' 105.7(13) . . ?
O18' S17' O19' 117.5(17) . . ?
O18' S17' N20' 114.1(14) . . ?
O19' S17' C13' 101.2(16) . . ?
O19' S17' N20' 113.1(16) . . ?
N20' S17' C13' 102.9(13) . . ?
S21' N20' S17' 131.0(14) . . ?
N20' S21' C24' 99.6(11) . . ?
O22' S21' N20' 115.5(14) . . ?
O22' S21' O23' 112.4(15) . . ?
O22' S21' C24' 105.4(12) . . ?
O23' S21' N20' 117.9(15) . . ?
O23' S21' C24' 103.4(13) . . ?
F25' C24' S21' 109.7(16) . . ?
F25' C24' F26' 107(2) . . ?
F26' C24' S21' 108.8(16) . . ?
F27' C24' S21' 113(2) . . ?
F27' C24' F25' 111(3) . . ?
F27' C24' F26' 107(3) . . ?

_database_code_depnum_ccdc_archive 'CCDC 1003259'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_nrb185
_audit_creation_date             2014-05-06
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            
;
 tetrakis(N-ethylimidazole) palladium(II) bistriflimide
;
_chemical_name_systematic        
;
 tetrakis(N-ethylimidazole) palladium(II) bis(trifluoromethyl)sulfonyl imide
;
_chemical_formula_moiety         'C20 H32 N8 Pd, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C24 H32 F12 N10 O8 Pd S4'
_chemical_formula_weight         1051.24
_chemical_melting_point          349
_chemical_oxdiff_formula         'Pd C4 F12 S4 O8 N2 N8 C20 H32'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   8.8459(5)
_cell_length_b                   9.1693(6)
_cell_length_c                   14.3228(9)
_cell_angle_alpha                92.776(5)
_cell_angle_beta                 106.337(5)
_cell_angle_gamma                113.370(6)
_cell_volume                     1006.34(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0640
_cell_measurement_theta_min      3.4460
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8744
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         2.92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0835511000
_diffrn_orient_matrix_UB_12      -0.0469677000
_diffrn_orient_matrix_UB_13      -0.0352484000
_diffrn_orient_matrix_UB_21      -0.0094602000
_diffrn_orient_matrix_UB_22      0.0715786000
_diffrn_orient_matrix_UB_23      -0.0097418000
_diffrn_orient_matrix_UB_31      0.0384443000
_diffrn_orient_matrix_UB_32      0.0037562000
_diffrn_orient_matrix_UB_33      -0.0376389000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                4371
_reflns_number_total             4580
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         4580
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0240
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0234P)²+0.6259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0581
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S34-C30 \\sim S38-C41 \\sim S19-C15 \\sim S23-C26
 with sigma of 0.01
3. Rigid bond restraints
 C30, F31, F32, F33, S34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
4. Others
 Fixed Sof: C15(0.5) F16(0.5) F17(0.5) F18(0.5) S19(0.5) O20(0.5) O21(0.5)
 N22(0.5) S23(0.5) O24(0.5) O25(0.5) C26(0.5) F27(0.5) F28(0.5) F29(0.5)
 C30(0.5) F31(0.5) F32(0.5) F33(0.5) S34(0.5) O35(0.5) O36(0.5) N37(0.5)
 S38(0.5) O39(0.5) O40(0.5) C41(0.5) F42(0.5) F43(0.5) F44(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 0.0000 0.5000 0.01556(5) Uani 1 d . . 2 S T P
N1 N 0.29891(16) -0.03005(16) 0.37872(10) 0.0188(3) Uani 1 d . . 1 . . .
C2 C 0.2891(2) -0.0646(2) 0.28557(12) 0.0202(3) Uani 1 d . . 1 . . .
H2 H 0.3768 -0.0789 0.2657 0.024 Uiso 1 calc . . 1 R . .
N3 N 0.13748(17) -0.07645(17) 0.22327(10) 0.0215(3) Uani 1 d . . 1 . . .
C4 C 0.0460(2) -0.0477(2) 0.27955(13) 0.0264(4) Uani 1 d . . 1 . . .
H4 H -0.0658 -0.0480 0.2559 0.032 Uiso 1 calc . . 1 R . .
C5 C 0.1466(2) -0.0189(2) 0.37559(13) 0.0263(4) Uani 1 d . . 1 . . .
H5 H 0.1170 0.0051 0.4314 0.032 Uiso 1 calc . . 1 R . .
C6 C 0.0789(2) -0.1168(3) 0.11467(13) 0.0306(4) Uani 1 d . . 1 . . .
H6A H 0.1818 -0.0823 0.0921 0.037 Uiso 1 calc . . 1 R . .
H6B H 0.0105 -0.0570 0.0861 0.037 Uiso 1 calc . . 1 R . .
C7 C -0.0309(3) -0.2945(3) 0.07804(17) 0.0534(6) Uani 1 d . . 1 . . .
H7A H -0.0668 -0.3173 0.0057 0.080 Uiso 1 calc . . 1 GR . .
H7B H -0.1344 -0.3285 0.0988 0.080 Uiso 1 calc . . 1 GR . .
H7C H 0.0369 -0.3540 0.1057 0.080 Uiso 1 calc . . 1 GR . .
N8 N 0.46561(17) 0.17493(17) 0.56975(10) 0.0188(3) Uani 1 d . . 1 . . .
C9 C 0.5567(2) 0.3323(2) 0.57879(11) 0.0183(3) Uani 1 d . . 1 . . .
H9 H 0.6465 0.3805 0.5510 0.022 Uiso 1 calc . . 1 R . .
N10 N 0.50410(18) 0.41428(17) 0.63292(10) 0.0207(3) Uani 1 d . . 1 . . .
C11 C 0.3729(2) 0.3029(2) 0.65964(15) 0.0315(4) Uani 1 d . . 1 . . .
H11 H 0.3105 0.3254 0.6982 0.038 Uiso 1 calc . . 1 R . .
C12 C 0.3493(2) 0.1555(2) 0.62065(15) 0.0305(4) Uani 1 d . . 1 . . .
H12 H 0.2666 0.0552 0.6271 0.037 Uiso 1 calc . . 1 R . .
C13 C 0.5773(3) 0.5904(2) 0.66100(14) 0.0276(4) Uani 1 d . . 1 . . .
H13A H 0.4836 0.6264 0.6375 0.033 Uiso 1 calc . . 1 R . .
H13B H 0.6656 0.6418 0.6286 0.033 Uiso 1 calc . . 1 R . .
C14 C 0.6611(3) 0.6442(2) 0.77217(15) 0.0378(5) Uani 1 d . . 1 . . .
H14A H 0.7116 0.7623 0.7886 0.057 Uiso 1 calc . . 1 GR . .
H14B H 0.7530 0.6076 0.7956 0.057 Uiso 1 calc . . 1 GR . .
H14C H 0.5727 0.5973 0.8042 0.057 Uiso 1 calc . . 1 GR . .
C15 C 0.5294(14) 1.2777(10) 0.9615(12) 0.048(3) Uani 0.50 d A -1 1 . . .
F16 F 0.4367(5) 1.3537(4) 0.9175(2) 0.0634(9) Uani 0.50 d A -1 1 . . .
F17 F 0.5771(8) 1.3160(6) 1.0567(4) 0.0708(14) Uani 0.50 d A -1 1 . . .
F18 F 0.6756(5) 1.3371(4) 0.9329(4) 0.0709(11) Uani 0.50 d A -1 1 . . .
S19 S 0.4106(5) 1.0603(6) 0.9151(3) 0.0221(5) Uani 0.50 d A -1 1 . . .
O20 O 0.2611(4) 1.0169(4) 0.9451(2) 0.0372(7) Uani 0.50 d A -1 1 . . .
O21 O 0.3880(4) 1.0476(4) 0.8116(2) 0.0369(6) Uani 0.50 d A -1 1 . . .
N22 N 0.5492(4) 0.9985(4) 0.9662(2) 0.0249(6) Uani 0.50 d A -1 1 . . .
S23 S 0.5563(6) 0.9224(6) 1.0639(3) 0.0247(6) Uani 0.50 d A -1 1 . . .
O24 O 0.4802(3) 0.9707(3) 1.12825(18) 0.0310(6) Uani 0.50 d A -1 1 . . .
O25 O 0.7263(4) 0.9310(5) 1.1045(3) 0.0489(9) Uani 0.50 d A -1 1 . . .
C26 C 0.4117(13) 0.7073(8) 1.0167(10) 0.041(2) Uani 0.50 d A -1 1 . . .
F27 F 0.2531(4) 0.6873(3) 0.9660(2) 0.0542(7) Uani 0.50 d A -1 1 . . .
F28 F 0.4061(7) 0.6271(4) 1.0884(3) 0.0704(12) Uani 0.50 d A -1 1 . . .
F29 F 0.4717(9) 0.6475(6) 0.9558(4) 0.0672(14) Uani 0.50 d A -1 1 . . .
C30 C -0.082(2) 0.420(2) 0.3090(9) 0.0208(17) Uani 0.50 d B -1 1 . U .
F31 F 0.0322(3) 0.5715(3) 0.31764(17) 0.0366(5) Uani 0.50 d B -1 1 . U .
F32 F -0.0570(4) 0.3229(3) 0.25379(17) 0.0397(6) Uani 0.50 d B -1 1 . U .
F33 F -0.2396(3) 0.4125(4) 0.27066(19) 0.0433(6) Uani 0.50 d B -1 1 . U .
S34 S -0.0584(12) 0.3587(11) 0.4299(8) 0.0228(10) Uani 0.50 d B -1 1 . U .
O35 O 0.0101(4) 0.2335(3) 0.4253(2) 0.0332(6) Uani 0.50 d B -1 1 . . .
O36 O -0.2284(3) 0.2904(3) 0.4466(2) 0.0293(6) Uani 0.50 d B -1 1 . . .
N37 N 0.0879(4) 0.5049(4) 0.5061(2) 0.0233(6) Uani 0.50 d B -1 1 . . .
S38 S 0.0563(13) 0.6462(12) 0.5609(7) 0.0210(9) Uani 0.50 d B -1 1 . . .
O39 O 0.1983(5) 0.7861(4) 0.5803(2) 0.0485(9) Uani 0.50 d B -1 1 . . .
O40 O -0.1194(4) 0.6231(3) 0.53240(19) 0.0315(6) Uani 0.50 d B -1 1 . . .
C41 C 0.093(3) 0.589(3) 0.6830(11) 0.032(3) Uani 0.50 d B -1 1 . . .
F42 F 0.1388(6) 0.4689(5) 0.6871(2) 0.0660(10) Uani 0.50 d B -1 1 . . .
F43 F -0.0485(3) 0.5437(4) 0.71287(18) 0.0429(6) Uani 0.50 d B -1 1 . . .
F44 F 0.2198(4) 0.7089(5) 0.7552(2) 0.0720(11) Uani 0.50 d B -1 1 . . .


_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
Pd1 N1 2.0208(13) 2_656 ?
Pd1 N1 2.0209(13) . ?
Pd1 N8 2.0165(13) 2_656 ?
Pd1 N8 2.0165(13) . ?
N1 C2 1.327(2) . ?
N1 C5 1.380(2) . ?
C2 N3 1.344(2) . ?
N3 C4 1.375(2) . ?
N3 C6 1.471(2) . ?
C4 C5 1.358(2) . ?
C6 C7 1.500(3) . ?
N8 C9 1.322(2) . ?
N8 C12 1.383(2) . ?
C9 N10 1.344(2) . ?
N10 C11 1.373(2) . ?
N10 C13 1.466(2) . ?
C11 C12 1.349(3) . ?
C13 C14 1.516(3) . ?
C15 F16 1.327(11) . ?
C15 F17 1.294(18) . ?
C15 F18 1.377(17) . ?
C15 S19 1.826(6) . ?
S19 O20 1.418(6) . ?
S19 O21 1.431(5) . ?
S19 N22 1.564(5) . ?
N22 S23 1.589(6) . ?
S23 O24 1.431(6) . ?
S23 O25 1.420(5) . ?
S23 C26 1.835(6) . ?
C26 F27 1.319(10) . ?
C26 F28 1.293(14) . ?
C26 F29 1.337(16) . ?
C30 F31 1.33(2) . ?
C30 F32 1.29(2) . ?
C30 F33 1.319(17) . ?
C30 S34 1.829(6) . ?
S34 O35 1.502(11) . ?
S34 O36 1.476(10) . ?
S34 N37 1.534(9) . ?
N37 S38 1.638(11) . ?
S38 O39 1.338(10) . ?
S38 O40 1.415(11) . ?
S38 C41 1.829(6) . ?
C41 F42 1.31(2) . ?
C41 F43 1.35(2) . ?
C41 F44 1.34(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
N1 Pd1 N1 179.999(1) 2_656 . ?
N8 Pd1 N1 90.54(5) 2_656 2_656 ?
N8 Pd1 N1 89.46(5) 2_656 . ?
N8 Pd1 N1 90.54(5) . . ?
N8 Pd1 N1 89.46(5) . 2_656 ?
N8 Pd1 N8 180.00(7) 2_656 . ?
C2 N1 Pd1 125.91(11) . . ?
C2 N1 C5 106.56(14) . . ?
C5 N1 Pd1 127.53(11) . . ?
N1 C2 N3 110.48(14) . . ?
C2 N3 C4 107.60(14) . . ?
C2 N3 C6 126.04(14) . . ?
C4 N3 C6 126.35(14) . . ?
C5 C4 N3 106.62(15) . . ?
C4 C5 N1 108.74(15) . . ?
N3 C6 C7 111.58(17) . . ?
C9 N8 Pd1 125.94(11) . . ?
C9 N8 C12 106.63(14) . . ?
C12 N8 Pd1 127.38(12) . . ?
N8 C9 N10 110.38(14) . . ?
C9 N10 C11 107.49(14) . . ?
C9 N10 C13 126.27(14) . . ?
C11 N10 C13 126.22(14) . . ?
C12 C11 N10 106.93(15) . . ?
C11 C12 N8 108.57(16) . . ?
N10 C13 C14 111.29(14) . . ?
F16 C15 F18 103.9(11) . . ?
F16 C15 S19 110.4(6) . . ?
F17 C15 F16 110.8(10) . . ?
F17 C15 F18 108.6(8) . . ?
F17 C15 S19 113.6(10) . . ?
F18 C15 S19 109.1(9) . . ?
O20 S19 C15 103.3(6) . . ?
O20 S19 O21 118.6(3) . . ?
O20 S19 N22 117.8(3) . . ?
O21 S19 C15 103.2(7) . . ?
O21 S19 N22 109.2(4) . . ?
N22 S19 C15 101.8(4) . . ?
S19 N22 S23 124.8(4) . . ?
N22 S23 C26 103.3(5) . . ?
O24 S23 N22 115.8(4) . . ?
O24 S23 C26 103.9(6) . . ?
O25 S23 N22 107.6(4) . . ?
O25 S23 O24 118.8(3) . . ?
O25 S23 C26 105.6(5) . . ?
F27 C26 S23 110.7(5) . . ?
F27 C26 F29 107.8(9) . . ?
F28 C26 S23 110.8(8) . . ?
F28 C26 F27 109.7(10) . . ?
F28 C26 F29 108.3(7) . . ?
F29 C26 S23 109.4(9) . . ?
F31 C30 S34 110.8(9) . . ?
F32 C30 F31 110.7(13) . . ?
F32 C30 F33 110.6(11) . . ?
F32 C30 S34 107.4(11) . . ?
F33 C30 F31 107.9(13) . . ?
F33 C30 S34 109.5(12) . . ?
O35 S34 C30 104.6(9) . . ?
O35 S34 N37 106.6(6) . . ?
O36 S34 C30 110.6(9) . . ?
O36 S34 O35 111.2(6) . . ?
O36 S34 N37 116.5(7) . . ?
N37 S34 C30 106.6(8) . . ?
S34 N37 S38 123.8(7) . . ?
N37 S38 C41 96.7(9) . . ?
O39 S38 N37 108.7(7) . . ?
O39 S38 O40 127.3(8) . . ?
O39 S38 C41 100.0(9) . . ?
O40 S38 N37 114.5(6) . . ?
O40 S38 C41 103.4(8) . . ?
F42 C41 S38 112.8(13) . . ?
F42 C41 F43 106.6(13) . . ?
F42 C41 F44 105.6(12) . . ?
F43 C41 S38 113.1(11) . . ?
F44 C41 S38 113.5(12) . . ?
F44 C41 F43 104.6(13) . . ?

_database_code_depnum_ccdc_archive 'CCDC 1003260'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_kb2019
_audit_creation_date             2014-05-06
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            
;
 bis(N-methylimidazole) bis(N-ethylimidazole) palladium(II) bistriflimide
;
_chemical_name_systematic        
;
  bis(N-methylimidazole) bis(N-ethylimidazole) palladium(II)
bis(trifluoromethyl)sulfonyl imide
;
_chemical_formula_moiety         'C18 H28 N8 Pd, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C22 H28 F12 N10 O8 Pd S4'
_chemical_formula_weight         1023.18
_chemical_melting_point          318
_chemical_oxdiff_formula         'Pd C18 N4 H28 C4 F12 N2 S4 O8'
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 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   10.2427(8)
_cell_length_b                   11.3109(5)
_cell_length_c                   15.6582(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.056(6)
_cell_angle_gamma                90.00
_cell_volume                     1814.07(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.394
_cell_measurement_theta_min      3.263
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9615
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.98
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0272066000
_diffrn_orient_matrix_UB_12      0.0420496000
_diffrn_orient_matrix_UB_13      -0.0284745000
_diffrn_orient_matrix_UB_21      0.0356803000
_diffrn_orient_matrix_UB_22      0.0254068000
_diffrn_orient_matrix_UB_23      0.0343211000
_diffrn_orient_matrix_UB_31      0.0526977000
_diffrn_orient_matrix_UB_32      -0.0389144000
_diffrn_orient_matrix_UB_33      -0.0083387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_number_gt                3503
_reflns_number_total             4200
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4200
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0365
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0376P)²+3.3950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0978
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C6, C6'}
{C13, C13'}
3. Restrained distances
 C6'-C7'
 1.5 with sigma of 0.01
 C13'-C14'
 1.5 with sigma of 0.01
4. Rigid bond restraints
 C6, C6', C7', C13, C13', C14'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C6 \\sim C6' \\sim C7' \\sim C13 \\sim C13' \\sim C14': within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C6) = Uanis(C6')
Uanis(C13) = Uanis(C13')
6. Others
 Fixed Sof: C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C6'(0.5) H6'A(0.5) H6'B(0.5)
 C7'(0.5) H7'A(0.5) H7'B(0.5) H7'C(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 C13'(0.5) H13D(0.5) H13E(0.5) C14'(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C6'(H6'A,H6'B), C13'(H13D,H13E)
7.b Me refined with riding coordinates:
 C7'(H7'A,H7'B,H7'C), C14'(H14A,H14B,H14C)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12)
7.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.0000 0.5000 0.5000 0.02289(10) Uani 1 d . . 2 S T P
N1 N 0.1832(3) 0.5321(2) 0.45932(15) 0.0254(5) Uani 1 d A . 1 . . .
C2 C 0.2453(3) 0.6345(3) 0.46174(19) 0.0288(7) Uani 1 d A . 1 . . .
H2 H 0.2075 0.7055 0.4786 0.035 Uiso 1 calc . . 1 R . .
N3 N 0.3693(3) 0.6230(2) 0.43686(18) 0.0337(6) Uani 1 d . . 1 . . .
C4 C 0.3881(3) 0.5061(3) 0.4162(2) 0.0354(7) Uani 1 d A . 1 . . .
H4 H 0.4648 0.4718 0.3963 0.042 Uiso 1 calc . . 1 R . .
C5 C 0.2734(3) 0.4511(3) 0.4306(2) 0.0297(7) Uani 1 d . . 1 . . .
H5 H 0.2578 0.3709 0.4225 0.036 Uiso 1 calc A . 1 R . .
C6 C 0.4671(4) 0.7164(4) 0.4347(4) 0.0685(15) Uani 0.50 d A 1 1 . U .
H6A H 0.4727 0.7479 0.3779 0.103 Uiso 0.50 calc A 1 1 GR . .
H6B H 0.5503 0.6847 0.4511 0.103 Uiso 0.50 calc A 1 1 GR . .
H6C H 0.4427 0.7782 0.4736 0.103 Uiso 0.50 calc A 1 1 GR . .
C6' C 0.4671(4) 0.7164(4) 0.4347(4) 0.0685(15) Uani 0.50 d A 2 1 D U .
H6'A H 0.4193 0.7871 0.4189 0.082 Uiso 0.50 calc A 2 1 R . .
H6'B H 0.4927 0.7275 0.4938 0.082 Uiso 0.50 calc A 2 1 R . .
C7' C 0.5849(14) 0.7228(17) 0.3879(13) 0.162(7) Uani 0.50 d A 2 1 D U .
H7'A H 0.6210 0.6449 0.3819 0.243 Uiso 0.50 calc A 2 1 R . .
H7'B H 0.6458 0.7725 0.4176 0.243 Uiso 0.50 calc A 2 1 R . .
H7'C H 0.5677 0.7553 0.3324 0.243 Uiso 0.50 calc A 2 1 R . .
N8 N -0.0574(3) 0.6564(2) 0.45163(15) 0.0244(5) Uani 1 d B . 1 . . .
C9 C -0.0944(3) 0.6738(2) 0.37161(18) 0.0241(6) Uani 1 d B . 1 . . .
H9 H -0.0995 0.6152 0.3301 0.029 Uiso 1 calc . . 1 R . .
N10 N -0.1236(3) 0.7881(2) 0.35907(16) 0.0276(6) Uani 1 d . . 1 . . .
C11 C -0.1043(3) 0.8462(3) 0.4354(2) 0.0318(7) Uani 1 d B . 1 . . .
H11 H -0.1173 0.9263 0.4458 0.038 Uiso 1 calc . . 1 R . .
C12 C -0.0627(3) 0.7644(3) 0.4925(2) 0.0298(7) Uani 1 d . . 1 . . .
H12 H -0.0414 0.7785 0.5494 0.036 Uiso 1 calc B . 1 R . .
C13 C -0.1673(4) 0.8409(3) 0.2789(2) 0.0382(8) Uani 0.50 d B 1 1 . U .
H13A H -0.1793 0.7799 0.2370 0.057 Uiso 0.50 calc B 1 1 GR . .
H13B H -0.1029 0.8961 0.2591 0.057 Uiso 0.50 calc B 1 1 GR . .
H13C H -0.2485 0.8814 0.2880 0.057 Uiso 0.50 calc B 1 1 GR . .
C13' C -0.1673(4) 0.8409(3) 0.2789(2) 0.0382(8) Uani 0.50 d B 2 1 D U .
H13D H -0.1597 0.7847 0.2324 0.046 Uiso 0.50 calc B 2 1 R . .
H13E H -0.1159 0.9104 0.2654 0.046 Uiso 0.50 calc B 2 1 R . .
C14' C -0.3056(10) 0.8732(15) 0.2933(11) 0.124(5) Uani 0.50 d B 2 1 D U .
H14A H -0.3606 0.8080 0.2776 0.186 Uiso 0.50 calc B 2 1 R . .
H14B H -0.3274 0.9408 0.2590 0.186 Uiso 0.50 calc B 2 1 R . .
H14C H -0.3185 0.8918 0.3525 0.186 Uiso 0.50 calc B 2 1 R . .
C15 C 0.7720(3) 0.1839(3) 0.2962(2) 0.0304(7) Uani 1 d . . 1 . . .
F16 F 0.8674(2) 0.14448(18) 0.24814(14) 0.0444(5) Uani 1 d . . 1 . . .
F17 F 0.6624(2) 0.1366(2) 0.26760(15) 0.0523(6) Uani 1 d . . 1 . . .
F18 F 0.7912(2) 0.14761(18) 0.37618(12) 0.0448(5) Uani 1 d . . 1 . . .
S19 S 0.76438(9) 0.34495(7) 0.29559(5) 0.03132(19) Uani 1 d . . 1 . . .
O20 O 0.6536(3) 0.3733(3) 0.34532(17) 0.0613(9) Uani 1 d . . 1 . . .
O21 O 0.8896(3) 0.3825(2) 0.32699(15) 0.0446(7) Uani 1 d . . 1 . . .
N22 N 0.7410(3) 0.3605(2) 0.19616(16) 0.0290(6) Uani 1 d . . 1 . . .
S23 S 0.77741(8) 0.47147(6) 0.14177(5) 0.02560(17) Uani 1 d . . 1 . . .
O24 O 0.7788(2) 0.4389(2) 0.05340(14) 0.0338(5) Uani 1 d . . 1 . . .
O25 O 0.8807(2) 0.5436(2) 0.17449(15) 0.0364(5) Uani 1 d . . 1 . . .
C26 C 0.6324(4) 0.5658(3) 0.1518(2) 0.0367(8) Uani 1 d . . 1 . . .
F27 F 0.6149(2) 0.59642(19) 0.23332(14) 0.0458(5) Uani 1 d . . 1 . . .
F28 F 0.5265(2) 0.5109(2) 0.12432(17) 0.0519(6) Uani 1 d . . 1 . . .
F29 F 0.6483(3) 0.66357(19) 0.10611(17) 0.0599(7) Uani 1 d . . 1 . . .


_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
Pd1 N1 2.015(3) 3_566 ?
Pd1 N1 2.015(3) . ?
Pd1 N8 2.012(2) . ?
Pd1 N8 2.012(2) 3_566 ?
N1 C2 1.323(4) . ?
N1 C5 1.377(4) . ?
C2 N3 1.335(4) . ?
N3 C4 1.374(4) . ?
N3 C6 1.457(5) . ?
C4 C5 1.349(5) . ?
N8 C9 1.324(4) . ?
N8 C12 1.380(4) . ?
C9 N10 1.342(4) . ?
N10 C11 1.379(4) . ?
N10 C13 1.459(4) . ?
C11 C12 1.355(4) . ?
C15 F16 1.312(4) . ?
C15 F17 1.321(4) . ?
C15 F18 1.332(3) . ?
C15 S19 1.823(3) . ?
S19 O20 1.414(3) . ?
S19 O21 1.437(3) . ?
S19 N22 1.585(3) . ?
N22 S23 1.562(3) . ?
S23 O24 1.432(2) . ?
S23 O25 1.430(2) . ?
S23 C26 1.835(4) . ?
C26 F27 1.334(4) . ?
C26 F28 1.322(4) . ?
C26 F29 1.328(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
N1 Pd1 N1 180.0 . 3_566 ?
N8 Pd1 N1 90.31(10) . 3_566 ?
N8 Pd1 N1 90.31(10) 3_566 . ?
N8 Pd1 N1 89.69(10) 3_566 3_566 ?
N8 Pd1 N1 89.69(10) . . ?
N8 Pd1 N8 180.0 3_566 . ?
C2 N1 Pd1 126.6(2) . . ?
C2 N1 C5 105.6(3) . . ?
C5 N1 Pd1 127.5(2) . . ?
N1 C2 N3 111.3(3) . . ?
C2 N3 C4 107.3(3) . . ?
C2 N3 C6 126.2(3) . . ?
C4 N3 C6 126.5(3) . . ?
C5 C4 N3 106.4(3) . . ?
C4 C5 N1 109.4(3) . . ?
C9 N8 Pd1 124.8(2) . . ?
C9 N8 C12 107.2(2) . . ?
C12 N8 Pd1 128.0(2) . . ?
N8 C9 N10 110.2(3) . . ?
C9 N10 C11 107.5(3) . . ?
C9 N10 C13 126.0(3) . . ?
C11 N10 C13 126.5(3) . . ?
C12 C11 N10 106.9(3) . . ?
C11 C12 N8 108.1(3) . . ?
F16 C15 F17 107.5(3) . . ?
F16 C15 F18 109.0(3) . . ?
F16 C15 S19 111.6(2) . . ?
F17 C15 F18 108.6(3) . . ?
F17 C15 S19 111.5(2) . . ?
F18 C15 S19 108.6(2) . . ?
O20 S19 C15 104.95(18) . . ?
O20 S19 O21 117.45(19) . . ?
O20 S19 N22 113.29(17) . . ?
O21 S19 C15 104.79(16) . . ?
O21 S19 N22 115.91(16) . . ?
N22 S19 C15 97.05(14) . . ?
S23 N22 S19 126.09(17) . . ?
N22 S23 C26 103.10(16) . . ?
O24 S23 N22 108.84(14) . . ?
O24 S23 C26 103.97(16) . . ?
O25 S23 N22 116.08(15) . . ?
O25 S23 O24 118.97(15) . . ?
O25 S23 C26 103.67(16) . . ?
F27 C26 S23 110.0(2) . . ?
F28 C26 S23 111.3(2) . . ?
F28 C26 F27 108.8(3) . . ?
F28 C26 F29 108.5(3) . . ?
F29 C26 S23 109.8(3) . . ?
F29 C26 F27 108.4(3) . . ?

_database_code_depnum_ccdc_archive 'CCDC 1003261'
