# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

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

data_R4
_database_code_depnum_ccdc_archive 'CCDC 1544212'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-07-27 downloaded from the CCDC.
;

#####################################################################
#                     CHEMICAL INFORMATION                          #
#####################################################################
_chemical_name_systematic        r4
_chemical_name_common            ?
_chemical_formula_moiety         'C17 H19 N3 O3 Pd S'
_chemical_formula_sum            'C17 H19 N3 O3 Pd S'
_chemical_formula_weight         451.81
_chemical_melting_point          ?
_chemical_compound_source        ?

#####################################################################
#                    UNIT CELL INFORMATION                          #
#####################################################################
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z+1/2
-x,-y,-z
x,-y-1/2,z-1/2

_cell_length_a                   8.3219(6)
_cell_length_b                   11.2480(9)
_cell_length_c                   18.4098(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.7126(11)
_cell_angle_gamma                90.00
_cell_volume                     1703.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      6.38
_cell_measurement_theta_max      22.52

#####################################################################
#                      CRYSTAL INFORMATION                          #
#####################################################################
_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_special_details           ?

#####################################################################
#                      ABSORPTION CORRECTION                        #
#####################################################################
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_T_max  0.946

#####################################################################
#                         DATA COLLECTION                           #
#####################################################################
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18317
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.24
_reflns_number_total             3076
_reflns_number_gt                2780
_reflns_threshold_expression     I>2σ(I)

#####################################################################
#                       COMPUTING PROGRAMS                          #
#####################################################################
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELX97-L (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

#####################################################################
#                     REFINEMENT INFORMATION                        #
#####################################################################
_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.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0498P)²+0.6722P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3076
_refine_ls_number_parameters     230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0766
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_details ?
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.095

#####################################################################
#      ATOMIC TYPES, COORDINATES AND DISPLACEMENT PARAMETERS        #
#####################################################################
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
O O 0.0106 0.0060 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.14935(2) 0.328085(17) 0.473094(10) 0.03141(10) Uani 1 1 d . . .
S1 S 0.24104(9) 0.19480(6) 0.56219(4) 0.03819(18) Uani 1 1 d . . .
O1 O 0.0084(3) 0.19402(17) 0.41942(12) 0.0478(5) Uani 1 1 d . . .
O2 O -0.2115(3) 0.12900(19) 0.34985(12) 0.0517(5) Uani 1 1 d . . .
O3 O 0.3768(3) 0.2174(2) 0.62178(14) 0.0657(7) Uani 1 1 d . . .
N1 N 0.0716(3) 0.44765(19) 0.39470(12) 0.0321(5) Uani 1 1 d . . .
N2 N 0.1274(3) 0.55542(19) 0.40413(12) 0.0351(5) Uani 1 1 d . . .
N3 N 0.5456(3) 0.6138(2) 0.66333(13) 0.0400(5) Uani 1 1 d . . .
C1 C -0.1085(4) 0.2067(3) 0.36533(15) 0.0379(6) Uani 1 1 d . . .
C2 C -0.1188(3) 0.3161(2) 0.31600(16) 0.0347(6) Uani 1 1 d . . .
C3 C -0.2274(4) 0.3051(3) 0.24995(17) 0.0411(7) Uani 1 1 d . . .
H3 H -0.2861 0.2349 0.2410 0.049 Uiso 1 1 calc R . .
C4 C -0.2501(4) 0.3937(3) 0.19826(16) 0.0452(7) Uani 1 1 d . . .
H4 H -0.3231 0.3831 0.1552 0.054 Uiso 1 1 calc R . .
C5 C -0.1649(4) 0.4982(3) 0.21027(16) 0.0429(7) Uani 1 1 d . . .
H5 H -0.1789 0.5581 0.1751 0.052 Uiso 1 1 calc R . .
C6 C -0.0584(3) 0.5142(3) 0.27457(15) 0.0394(6) Uani 1 1 d . . .
H6 H -0.0010 0.5852 0.2823 0.047 Uiso 1 1 calc R . .
C7 C -0.0356(3) 0.4254(2) 0.32834(14) 0.0315(5) Uani 1 1 d . . .
C8 C 0.2323(3) 0.5685(2) 0.46752(15) 0.0338(6) Uani 1 1 d . . .
C9 C 0.3032(4) 0.6800(2) 0.48546(17) 0.0394(7) Uani 1 1 d . . .
H9 H 0.2788 0.7440 0.4537 0.047 Uiso 1 1 calc R . .
C10 C 0.4083(4) 0.6948(3) 0.54975(17) 0.0394(6) Uani 1 1 d . . .
H10 H 0.4558 0.7687 0.5610 0.047 Uiso 1 1 calc R . .
C11 C 0.4452(3) 0.5992(2) 0.59901(14) 0.0343(6) Uani 1 1 d . . .
C12 C 0.3748(3) 0.4852(2) 0.57956(14) 0.0342(6) Uani 1 1 d . . .
H12 H 0.4010 0.4210 0.6109 0.041 Uiso 1 1 calc R . .
C13 C 0.2697(3) 0.4693(2) 0.51563(14) 0.0321(6) Uani 1 1 d . . .
C14 C 0.5903(4) 0.5161(3) 0.71402(17) 0.0498(7) Uani 1 1 d . . .
H14A H 0.6462 0.4563 0.6903 0.075 Uiso 1 1 calc R . .
H14B H 0.4940 0.4826 0.7286 0.075 Uiso 1 1 calc R . .
H14C H 0.6602 0.5450 0.7566 0.075 Uiso 1 1 calc R . .
C15 C 0.6157(4) 0.7292(3) 0.68494(18) 0.0516(8) Uani 1 1 d . . .
H15A H 0.5312 0.7879 0.6808 0.077 Uiso 1 1 calc R . .
H15B H 0.6932 0.7502 0.6534 0.077 Uiso 1 1 calc R . .
H15C H 0.6692 0.7256 0.7349 0.077 Uiso 1 1 calc R . .
C16 C 0.0706(4) 0.1499(3) 0.6019(2) 0.0557(9) Uani 1 1 d . . .
H16A H 0.0387 0.2132 0.6316 0.084 Uiso 1 1 calc R . .
H16B H 0.0982 0.0809 0.6320 0.084 Uiso 1 1 calc R . .
H16C H -0.0176 0.1311 0.5637 0.084 Uiso 1 1 calc R . .
C17 C 0.2828(5) 0.0600(3) 0.5181(2) 0.0606(9) Uani 1 1 d . . .
H17A H 0.2939 -0.0036 0.5532 0.091 Uiso 1 1 calc R . .
H17B H 0.3819 0.0683 0.4978 0.091 Uiso 1 1 calc R . .
H17C H 0.1950 0.0426 0.4794 0.091 Uiso 1 1 calc R . .


#####################################################################
#                       MOLECULAR GEOMETRY                          #
#####################################################################
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 C13 1.976(3) . ?
Pd1 N1 2.007(2) . ?
Pd1 O1 2.068(2) . ?
Pd1 S1 2.2674(7) . ?
S1 O3 1.473(2) . ?
S1 C16 1.765(3) . ?
S1 C17 1.779(3) . ?
O1 C1 1.290(3) . ?
O2 C1 1.227(4) . ?
N1 N2 1.300(3) . ?
N1 C7 1.422(3) . ?
N2 C8 1.355(3) . ?
N3 C11 1.352(3) . ?
N3 C15 1.453(4) . ?
N3 C14 1.453(4) . ?
C1 C2 1.524(4) . ?
C2 C3 1.407(4) . ?
C2 C7 1.412(4) . ?
C3 C4 1.372(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.399(4) . ?
C6 H6 0.9300 . ?
C8 C9 1.404(4) . ?
C8 C13 1.429(4) . ?
C9 C10 1.371(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.410(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.432(4) . ?
C12 C13 1.368(4) . ?
C12 H12 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Pd1 N1 80.50(10) . . ?
C13 Pd1 O1 173.12(9) . . ?
N1 Pd1 O1 92.72(8) . . ?
C13 Pd1 S1 98.63(8) . . ?
N1 Pd1 S1 179.03(6) . . ?
O1 Pd1 S1 88.16(6) . . ?
O3 S1 C16 108.34(17) . . ?
O3 S1 C17 107.83(18) . . ?
C16 S1 C17 99.77(18) . . ?
O3 S1 Pd1 124.13(10) . . ?
C16 S1 Pd1 106.60(12) . . ?
C17 S1 Pd1 107.50(12) . . ?
C1 O1 Pd1 126.51(18) . . ?
N2 N1 C7 116.4(2) . . ?
N2 N1 Pd1 117.33(16) . . ?
C7 N1 Pd1 126.29(17) . . ?
N1 N2 C8 112.7(2) . . ?
C11 N3 C15 121.2(2) . . ?
C11 N3 C14 122.3(2) . . ?
C15 N3 C14 116.5(2) . . ?
O2 C1 O1 121.3(3) . . ?
O2 C1 C2 117.6(3) . . ?
O1 C1 C2 121.1(3) . . ?
C3 C2 C7 116.8(2) . . ?
C3 C2 C1 114.5(2) . . ?
C7 C2 C1 128.7(3) . . ?
C4 C3 C2 122.6(3) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 121.0(3) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C2 119.8(2) . . ?
C6 C7 N1 118.9(2) . . ?
C2 C7 N1 121.3(2) . . ?
N2 C8 C9 119.5(2) . . ?
N2 C8 C13 120.0(2) . . ?
C9 C8 C13 120.5(2) . . ?
C10 C9 C8 120.1(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 120.7(2) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
N3 C11 C10 121.0(2) . . ?
N3 C11 C12 120.2(2) . . ?
C10 C11 C12 118.7(2) . . ?
C13 C12 C11 121.1(2) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C8 118.8(2) . . ?
C12 C13 Pd1 131.8(2) . . ?
C8 C13 Pd1 109.41(18) . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
S1 C17 H17A 109.5 . . ?
S1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
S1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

#####################################################################
#                  SHELXL-97  instruction file (.INS)               #
#                 used in the last cycles of refinement             #
#####################################################################
_iucr_refine_instruction_details 
;
TITL R4 - P21/c
CELL 0.71073 8.3219 11.2480 18.4098 90.00 98.7126 90.00
ZERR    4    0.0006  0.0009  0.0014  0.00  0.0011 0.00
LATT  1
SYMM -X, 0.50000+Y, 0.50000-Z
SFAC C  H  N  O  PD  S
UNIT 68 76 12 12  4  4
REM  Crystal colour: (metallic) black
SIZE  0.17 0.10 0.05
TEMP  22
OMIT  -2 50.5
MERG  2
L.S.  15
FMAP  2
PLAN  25
BOND  $H
ACTA
WGHT    0.049800    0.672200
FVAR       0.28108
PD1     5   0.14935   0.32809   0.47309  11.00000   0.03303   0.02708 =
        0.03330   0.00397   0.00238  -0.00035
S1      6   0.24104   0.19480   0.56219  11.00000   0.03721   0.03374 =
        0.04195   0.01047   0.00064  -0.00176
O1      4   0.00840   0.19402   0.41942  11.00000   0.05721   0.03097 =
        0.04977   0.00437  -0.00939  -0.00594
O2      4  -0.21148   0.12900   0.34985  11.00000   0.05834   0.03972 =
        0.05349   0.00393  -0.00281  -0.01470
O3      4   0.37681   0.21736   0.62178  11.00000   0.06224   0.05602 =
        0.06721   0.02392  -0.02725  -0.01400
N1      3   0.07163   0.44765   0.39470  11.00000   0.03168   0.03043 =
        0.03407   0.00300   0.00506   0.00145
N2      3   0.12742   0.55542   0.40413  11.00000   0.03712   0.02940 =
        0.03808   0.00327   0.00372   0.00104
N3      3   0.54559   0.61384   0.66333  11.00000   0.04096   0.03832 =
        0.03888  -0.00280   0.00026  -0.00427
C1      1  -0.10847   0.20670   0.36533  11.00000   0.04476   0.03200 =
        0.03758  -0.00381   0.00803   0.00073
C2      1  -0.11876   0.31614   0.31600  11.00000   0.03390   0.03585 =
        0.03505  -0.00137   0.00788   0.00462
C3      1  -0.22740   0.30507   0.24995  11.00000   0.03937   0.04025 =
        0.04270  -0.00743   0.00280  -0.00419
AFIX  43
H3      2  -0.28612   0.23488   0.24098  11.00000  -1.20000
AFIX   0
C4      1  -0.25013   0.39372   0.19826  11.00000   0.04308   0.05591 =
        0.03409  -0.00382  -0.00244   0.00527
AFIX  43
H4      2  -0.32306   0.38312   0.15521  11.00000  -1.20000
AFIX   0
C5      1  -0.16485   0.49819   0.21027  11.00000   0.04561   0.04316 =
        0.03895   0.00649   0.00300   0.01046
AFIX  43
H5      2  -0.17889   0.55809   0.17506  11.00000  -1.20000
AFIX   0
C6      1  -0.05842   0.51423   0.27457  11.00000   0.04040   0.03752 =
        0.03909   0.00388   0.00246   0.00062
AFIX  43
H6      2  -0.00096   0.58516   0.28232  11.00000  -1.20000
AFIX   0
C7      1  -0.03555   0.42539   0.32834  11.00000   0.02952   0.03345 =
        0.03151  -0.00060   0.00480   0.00474
C8      1   0.23226   0.56851   0.46752  11.00000   0.03509   0.03025 =
        0.03579   0.00264   0.00475   0.00233
C9      1   0.30317   0.68004   0.48546  11.00000   0.04396   0.03147 =
        0.04134   0.00541   0.00167   0.00128
AFIX  43
H9      2   0.27879   0.74399   0.45368  11.00000  -1.20000
AFIX   0
C10     1   0.40830   0.69481   0.54975  11.00000   0.03882   0.02978 =
        0.04858  -0.00308   0.00316  -0.00367
AFIX  43
H10     2   0.45579   0.76870   0.56100  11.00000  -1.20000
AFIX   0
C11     1   0.44518   0.59918   0.59901  11.00000   0.03006   0.03824 =
        0.03502  -0.00377   0.00641   0.00063
C12     1   0.37482   0.48524   0.57956  11.00000   0.03609   0.03134 =
        0.03486   0.00402   0.00452  -0.00085
AFIX  43
H12     2   0.40104   0.42099   0.61091  11.00000  -1.20000
AFIX   0
C13     1   0.26970   0.46933   0.51563  11.00000   0.03317   0.02870 =
        0.03536   0.00016   0.00771  -0.00011
C14     1   0.59029   0.51612   0.71402  11.00000   0.05139   0.05175 =
        0.04261   0.00352  -0.00441   0.00031
AFIX 137
H14A    2   0.64618   0.45625   0.69033  11.00000  -1.50000
H14B    2   0.49399   0.48256   0.72857  11.00000  -1.50000
H14C    2   0.66022   0.54501   0.75664  11.00000  -1.50000
AFIX   0
C15     1   0.61575   0.72918   0.68494  11.00000   0.05359   0.04991 =
        0.04803  -0.00804  -0.00295  -0.00742
AFIX 137
H15A    2   0.53117   0.78793   0.68079  11.00000  -1.50000
H15B    2   0.69319   0.75024   0.65341  11.00000  -1.50000
H15C    2   0.66924   0.72557   0.73490  11.00000  -1.50000
AFIX   0
C16     1   0.07065   0.14986   0.60191  11.00000   0.05430   0.05514 =
        0.06068   0.01957   0.01836   0.00292
AFIX 137
H16A    2   0.03867   0.21317   0.63165  11.00000  -1.50000
H16B    2   0.09820   0.08091   0.63196  11.00000  -1.50000
H16C    2  -0.01761   0.13107   0.56374  11.00000  -1.50000
AFIX   0
C17     1   0.28275   0.06000   0.51806  11.00000   0.07277   0.04249 =
        0.06938   0.01097   0.02002   0.01882
AFIX 137
H17A    2   0.29388  -0.00365   0.55321  11.00000  -1.50000
H17B    2   0.38189   0.06828   0.49781  11.00000  -1.50000
H17C    2   0.19500   0.04263   0.47936  11.00000  -1.50000
HKLF      4
REM  R4 - P21/c
REM R1 =  0.0275 for   2780 Fo > 4sig(Fo)  and  0.0307 for all   3076 data
REM    230 parameters refined using      0 restraints
END
WGHT      0.0496      0.6886
REM Highest difference peak  0.844,  deepest hole -0.438,  1-sigma level  0.095
Q1      0   0.17700   0.25280   0.51240  11.00000   0.05000   0.84000 =
        0.00000   0.00000   0.00000   0.00000
Q2      0   0.17370   0.39780   0.50790  11.00000   0.05000   0.83000 =
        0.00000   0.00000   0.00000   0.00000
Q3      0   0.15230   0.24370   0.47910  11.00000   0.05000   0.82000 =
        0.00000   0.00000   0.00000   0.00000
Q4      0   0.15570   0.41040   0.48520  11.00000   0.05000   0.80000 =
        0.00000   0.00000   0.00000   0.00000
Q5      0   0.12500   0.39970   0.43610  11.00000   0.05000   0.75000 =
        0.00000   0.00000   0.00000   0.00000
Q6      0   0.10950   0.30270   0.42230  11.00000   0.05000   0.68000 =
        0.00000   0.00000   0.00000   0.00000
Q7      0   0.23840   0.12320   0.53390  11.00000   0.05000   0.38000 =
        0.00000   0.00000   0.00000   0.00000
Q8      0   0.01910   0.44180   0.37090  11.00000   0.05000   0.38000 =
        0.00000   0.00000   0.00000   0.00000
Q9      0   0.08000   0.22120   0.39950  11.00000   0.05000   0.38000 =
        0.00000   0.00000   0.00000   0.00000
Q10     0   0.28860   0.20870   0.61850  11.00000   0.05000   0.37000 =
        0.00000   0.00000   0.00000   0.00000
Q11     0   0.49730   0.59660   0.63030  11.00000   0.05000   0.37000 =
        0.00000   0.00000   0.00000   0.00000
Q12     0   0.17840   0.56510   0.44960  11.00000   0.05000   0.36000 =
        0.00000   0.00000   0.00000   0.00000
Q13     0   0.24860   0.52150   0.49750  11.00000   0.05000   0.35000 =
        0.00000   0.00000   0.00000   0.00000
Q14     0  -0.11440   0.27740   0.34490  11.00000   0.05000   0.35000 =
        0.00000   0.00000   0.00000   0.00000
Q15     0  -0.16180   0.32170   0.28950  11.00000   0.05000   0.35000 =
        0.00000   0.00000   0.00000   0.00000
Q16     0   0.36880   0.68210   0.51560  11.00000   0.05000   0.32000 =
        0.00000   0.00000   0.00000   0.00000
Q17     0   0.12110   0.45300   0.38950  11.00000   0.05000   0.31000 =
        0.00000   0.00000   0.00000   0.00000
Q18     0  -0.09090   0.48850   0.23500  11.00000   0.05000   0.30000 =
        0.00000   0.00000   0.00000   0.00000
Q19     0  -0.00830   0.23990   0.43320  11.00000   0.05000   0.30000 =
        0.00000   0.00000   0.00000   0.00000
Q20     0  -0.04740   0.48130   0.30110  11.00000   0.05000   0.29000 =
        0.00000   0.00000   0.00000   0.00000
Q21     0   0.24510   0.45510   0.55070  11.00000   0.05000   0.28000 =
        0.00000   0.00000   0.00000   0.00000
Q22     0   0.31770   0.47940   0.54280  11.00000   0.05000   0.28000 =
        0.00000   0.00000   0.00000   0.00000
Q23     0   0.43200   0.55180   0.59220  11.00000   0.05000   0.25000 =
        0.00000   0.00000   0.00000   0.00000
Q24     0  -0.15070   0.43500   0.19910  11.00000   0.05000   0.25000 =
        0.00000   0.00000   0.00000   0.00000
Q25     0  -0.08460   0.37130   0.32430  11.00000   0.05000   0.24000 =
        0.00000   0.00000   0.00000   0.00000
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMSO-Ether'
