# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_3-lut
_database_code_depnum_ccdc_archive 'CCDC 1879934'
_audit_update_record             
;
2018-11-20 deposited with the CCDC.
2019-01-07 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
Refinement proceded smoothly.
;
_cell_length_a                   16.706(4)
_cell_length_b                   10.745(2)
_cell_length_c                   17.859(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.827(5)
_cell_angle_gamma                90
_cell_volume                     3125.7(12)

_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,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

_chemical_formula_sum            'C36 H38 N4 O5 Pd1'
_chemical_formula_moiety         'C32 H30 N4 O4 Pd1, C4 H8 O1'
_chemical_compound_source        synthesized
_chemical_formula_weight         713.12


_cell_measurement_reflns_used    9895
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.51
_cell_measurement_temperature    90

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.16
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_max          0.34

_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    0.645

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

_computing_data_collection       'Apex2, (Bruker, 2007)'
_computing_cell_refinement       'Apex2, (Bruker, 2007)'
_computing_data_reduction        'Apex2, (Bruker, 2007)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0

_diffrn_ambient_temperature      90
_diffrn_reflns_number            30358
_reflns_number_total             7166
_diffrn_reflns_av_R_equivalents  0.038


_diffrn_reflns_theta_min         1.250
_diffrn_reflns_theta_max         27.525
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        27.525
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -21
_reflns_limit_h_max              21
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_oxford_diffrn_Wilson_B_factor   0.95
_oxford_diffrn_Wilson_scale      87.44

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.84
_refine_diff_density_max         0.90


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         7136
_refine_ls_number_restraints     0
_refine_ls_number_parameters     415
_oxford_refine_ls_R_factor_ref   0.0375
_refine_ls_wR_factor_ref         0.0742
_refine_ls_goodness_of_fit_ref   0.9248
_refine_ls_shift/su_max          0.0020574
_refine_ls_shift/su_mean         0.0000347


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7136
_refine_ls_R_factor_all          0.0375
_refine_ls_wR_factor_all         0.0742

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5966
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_gt          0.0686

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 3.50 4.76 2.02 0.495 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.88796(15) 0.3236(2) 0.44040(14) 0.0193 1.0000 Uani . . . . . .
C2 C 0.88143(15) 0.2308(2) 0.50121(14) 0.0179 1.0000 Uani . . . . . .
O3 O 0.95316(10) 0.23773(16) 0.56481(9) 0.0166 1.0000 Uani . . . . . .
C4 C 0.94471(14) 0.3178(2) 0.62348(13) 0.0150 1.0000 Uani . . . . . .
C5 C 0.98900(14) 0.4273(2) 0.63557(14) 0.0180 1.0000 Uani . . . . . .
C6 C 0.97693(14) 0.5105(2) 0.69231(14) 0.0183 1.0000 Uani . . . . . .
C7 C 0.92133(14) 0.4840(2) 0.73771(13) 0.0154 1.0000 Uani . . . . . .
C8 C 0.88159(15) 0.3691(2) 0.72863(14) 0.0186 1.0000 Uani . . . . . .
C9 C 0.89218(16) 0.2868(2) 0.67137(14) 0.0184 1.0000 Uani . . . . . .
C10 C 0.89744(14) 0.5805(2) 0.79127(13) 0.0167 1.0000 Uani . . . . . .
N11 N 0.80791(12) 0.59430(19) 0.77638(11) 0.0143 1.0000 Uani . . . . . .
C12 C 0.76865(15) 0.5292(2) 0.82187(13) 0.0167 1.0000 Uani . . . . . .
O13 O 0.79916(12) 0.46176(18) 0.87737(10) 0.0242 1.0000 Uani . . . . . .
C14 C 0.67627(15) 0.5426(2) 0.79865(13) 0.0146 1.0000 Uani . . . . . .
C15 C 0.61873(16) 0.4838(2) 0.83201(14) 0.0181 1.0000 Uani . . . . . .
C16 C 0.53625(16) 0.5083(2) 0.80280(15) 0.0197 1.0000 Uani . . . . . .
C17 C 0.51123(14) 0.5913(2) 0.74159(14) 0.0177 1.0000 Uani . . . . . .
C18 C 0.57165(14) 0.6449(2) 0.70956(13) 0.0143 1.0000 Uani . . . . . .
N19 N 0.65067(12) 0.61861(18) 0.73895(11) 0.0122 1.0000 Uani . . . . . .
C20 C 0.55773(14) 0.7266(2) 0.63927(13) 0.0143 1.0000 Uani . . . . . .
O21 O 0.48657(11) 0.75523(17) 0.60553(11) 0.0206 1.0000 Uani . . . . . .
N22 N 0.62818(12) 0.75665(18) 0.61853(11) 0.0138 1.0000 Uani . . . . . .
C23 C 0.62081(14) 0.8187(2) 0.54396(13) 0.0159 1.0000 Uani . . . . . .
C24 C 0.63167(14) 0.7260(2) 0.48245(13) 0.0154 1.0000 Uani . . . . . .
C25 C 0.68591(15) 0.7497(2) 0.43510(13) 0.0169 1.0000 Uani . . . . . .
C26 C 0.70322(15) 0.6590(2) 0.38514(13) 0.0175 1.0000 Uani . . . . . .
C27 C 0.66752(14) 0.5422(2) 0.38393(13) 0.0157 1.0000 Uani . . . . . .
C28 C 0.60964(14) 0.5188(2) 0.42797(13) 0.0165 1.0000 Uani . . . . . .
C29 C 0.59198(14) 0.6109(2) 0.47641(13) 0.0163 1.0000 Uani . . . . . .
O30 O 0.68809(10) 0.44937(17) 0.33757(9) 0.0174 1.0000 Uani . . . . . .
C31 C 0.73602(15) 0.3484(2) 0.37910(14) 0.0180 1.0000 Uani . . . . . .
C32 C 0.82634(15) 0.3726(2) 0.38866(14) 0.0191 1.0000 Uani . . . . . .
C33 C 0.80532(14) 0.5602(2) 0.55948(13) 0.0160 1.0000 Uani . . . . . .
C34 C 0.83821(13) 0.6895(2) 0.57361(13) 0.0133 1.0000 Uani . . . . . .
C35 C 0.88956(15) 0.7410(2) 0.53040(14) 0.0177 1.0000 Uani . . . . . .
C36 C 0.91816(15) 0.8616(2) 0.54503(15) 0.0204 1.0000 Uani . . . . . .
C37 C 0.89584(15) 0.9281(2) 0.60361(14) 0.0182 1.0000 Uani . . . . . .
C38 C 0.84423(14) 0.8738(2) 0.64560(13) 0.0148 1.0000 Uani . . . . . .
N39 N 0.81580(11) 0.75614(18) 0.63014(11) 0.0120 1.0000 Uani . . . . . .
C40 C 0.81745(16) 0.9406(2) 0.70949(14) 0.0195 1.0000 Uani . . . . . .
C41 C 0.61273(19) 0.1439(3) 0.61223(19) 0.0334 1.0000 Uani . . . . . .
C42 C 0.6365(3) 0.2515(4) 0.6673(2) 0.0500 1.0000 Uani . . . . . .
C43 C 0.6594(2) 0.3517(3) 0.61962(19) 0.0348 1.0000 Uani . . . . . .
O44 O 0.69808(15) 0.2879(2) 0.56476(13) 0.0359 1.0000 Uani . . . . . .
C45 C 0.66617(18) 0.1638(3) 0.55266(15) 0.0270 1.0000 Uani . . . . . .
Pd1 Pd 0.732017(10) 0.685345(15) 0.687683(9) 0.0099 1.0000 Uani . . . . . .
H101 H 0.9162 0.5546 0.8428 0.0194 1.0000 Uiso . . . . . .
H102 H 0.9216 0.6604 0.7838 0.0201 1.0000 Uiso . . . . . .
H61 H 1.0058 0.5863 0.6994 0.0220 1.0000 Uiso . . . . . .
H51 H 1.0253 0.4461 0.6050 0.0218 1.0000 Uiso . . . . . .
H22 H 0.8805 0.1487 0.4792 0.0215 1.0000 Uiso . . . . . .
H21 H 0.8325 0.2447 0.5199 0.0203 1.0000 Uiso . . . . . .
H11 H 0.9410 0.3486 0.4389 0.0230 1.0000 Uiso . . . . . .
H321 H 0.8396 0.4286 0.3528 0.0232 1.0000 Uiso . . . . . .
H311 H 0.7218 0.3370 0.4281 0.0220 1.0000 Uiso . . . . . .
H312 H 0.7209 0.2757 0.3473 0.0212 1.0000 Uiso . . . . . .
H281 H 0.5844 0.4410 0.4251 0.0197 1.0000 Uiso . . . . . .
H291 H 0.5542 0.5947 0.5060 0.0205 1.0000 Uiso . . . . . .
H231 H 0.6636 0.8820 0.5495 0.0187 1.0000 Uiso . . . . . .
H232 H 0.5678 0.8584 0.5297 0.0196 1.0000 Uiso . . . . . .
H251 H 0.7118 0.8267 0.4381 0.0202 1.0000 Uiso . . . . . .
H261 H 0.7394 0.6750 0.3538 0.0208 1.0000 Uiso . . . . . .
H91 H 0.8628 0.2121 0.6647 0.0215 1.0000 Uiso . . . . . .
H81 H 0.8463 0.3492 0.7613 0.0223 1.0000 Uiso . . . . . .
H151 H 0.6354 0.4285 0.8721 0.0227 1.0000 Uiso . . . . . .
H161 H 0.4972 0.4693 0.8240 0.0241 1.0000 Uiso . . . . . .
H171 H 0.4564 0.6096 0.7218 0.0212 1.0000 Uiso . . . . . .
H332 H 0.8281 0.5227 0.5200 0.0238 1.0000 Uiso . . . . . .
H333 H 0.8195 0.5115 0.6049 0.0240 1.0000 Uiso . . . . . .
H331 H 0.7462 0.5628 0.5434 0.0236 1.0000 Uiso . . . . . .
H351 H 0.9037 0.6946 0.4909 0.0216 1.0000 Uiso . . . . . .
H361 H 0.9521 0.8969 0.5163 0.0243 1.0000 Uiso . . . . . .
H371 H 0.9151 1.0086 0.6151 0.0223 1.0000 Uiso . . . . . .
H401 H 0.8403 1.0226 0.7150 0.0300 1.0000 Uiso . . . . . .
H402 H 0.8351 0.8959 0.7570 0.0295 1.0000 Uiso . . . . . .
H403 H 0.7588 0.9479 0.6990 0.0287 1.0000 Uiso . . . . . .
H452 H 0.7090 0.1088 0.5601 0.0319 1.0000 Uiso . . . . . .
H451 H 0.6325 0.1567 0.5020 0.0329 1.0000 Uiso . . . . . .
H411 H 0.6263 0.0643 0.6382 0.0402 1.0000 Uiso . . . . . .
H412 H 0.5543 0.1492 0.5871 0.0404 1.0000 Uiso . . . . . .
H432 H 0.6977 0.4096 0.6504 0.0423 1.0000 Uiso . . . . . .
H431 H 0.6116 0.3932 0.5936 0.0425 1.0000 Uiso . . . . . .
H421 H 0.6837 0.2306 0.7097 0.0612 1.0000 Uiso . . . . . .
H422 H 0.5906 0.2783 0.6873 0.0604 1.0000 Uiso . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.10728(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.496(3) yes
C1 . C32 . 1.330(4) yes
C1 . H11 . 0.932 no
C2 . O3 . 1.459(3) yes
C2 . H22 . 0.964 no
C2 . H21 . 0.960 no
O3 . C4 . 1.387(3) yes
C4 . C5 . 1.381(3) yes
C4 . C9 . 1.395(3) yes
C5 . C6 . 1.399(3) yes
C5 . H51 . 0.925 no
C6 . C7 . 1.391(3) yes
C6 . H61 . 0.941 no
C7 . C8 . 1.395(4) yes
C7 . C10 . 1.523(3) yes
C8 . C9 . 1.392(3) yes
C8 . H81 . 0.941 no
C9 . H91 . 0.934 no
C10 . N11 . 1.467(3) yes
C10 . H101 . 0.946 no
C10 . H102 . 0.970 no
N11 . C12 . 1.348(3) yes
N11 . Pd1 . 2.045(2) yes
C12 . O13 . 1.242(3) yes
C12 . C14 . 1.514(3) yes
C14 . C15 . 1.390(3) yes
C14 . N19 . 1.336(3) yes
C14 . Pd1 . 2.822(2) yes
C15 . C16 . 1.386(4) yes
C15 . H151 . 0.925 no
C16 . C17 . 1.401(4) yes
C16 . H161 . 0.923 no
C17 . C18 . 1.391(3) yes
C17 . H171 . 0.927 no
C18 . N19 . 1.338(3) yes
C18 . C20 . 1.507(3) yes
C18 . Pd1 . 2.826(2) yes
N19 . Pd1 . 1.9370(19) yes
C20 . O21 . 1.246(3) yes
C20 . N22 . 1.349(3) yes
N22 . C23 . 1.470(3) yes
N22 . Pd1 . 2.042(2) yes
C23 . C24 . 1.523(3) yes
C23 . H231 . 0.975 no
C23 . H232 . 0.965 no
C24 . C25 . 1.393(3) yes
C24 . C29 . 1.397(3) yes
C25 . C26 . 1.394(3) yes
C25 . H251 . 0.930 no
C26 . C27 . 1.387(3) yes
C26 . H261 . 0.926 no
C27 . C28 . 1.398(3) yes
C27 . O30 . 1.388(3) yes
C28 . C29 . 1.389(3) yes
C28 . H281 . 0.933 no
C29 . H291 . 0.926 no
O30 . C31 . 1.451(3) yes
C31 . C32 . 1.503(3) yes
C31 . H311 . 0.965 no
C31 . H312 . 0.965 no
C32 . H321 . 0.941 no
C33 . C34 . 1.495(3) yes
C33 . H332 . 0.960 no
C33 . H333 . 0.950 no
C33 . H331 . 0.965 no
C34 . C35 . 1.389(3) yes
C34 . N39 . 1.356(3) yes
C35 . C36 . 1.386(4) yes
C35 . H351 . 0.935 no
C36 . C37 . 1.385(4) yes
C36 . H361 . 0.925 no
C37 . C38 . 1.391(3) yes
C37 . H371 . 0.930 no
C38 . N39 . 1.357(3) yes
C38 . C40 . 1.498(3) yes
N39 . Pd1 . 2.0572(19) yes
C40 . H401 . 0.956 no
C40 . H402 . 0.962 no
C40 . H403 . 0.959 no
C41 . C42 . 1.512(5) yes
C41 . C45 . 1.548(4) yes
C41 . H411 . 0.976 no
C41 . H412 . 0.981 no
C42 . C43 . 1.475(4) yes
C42 . H421 . 0.990 no
C42 . H422 . 0.960 no
C43 . O44 . 1.458(4) yes
C43 . H432 . 0.970 no
C43 . H431 . 0.944 no
O44 . C45 . 1.435(3) yes
C45 . H452 . 0.914 no
C45 . H451 . 0.956 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C32 . 126.7(2) yes
C2 . C1 . H11 . 115.9 no
C32 . C1 . H11 . 117.4 no
C1 . C2 . O3 . 110.6(2) yes
C1 . C2 . H22 . 108.1 no
O3 . C2 . H22 . 107.4 no
C1 . C2 . H21 . 110.7 no
O3 . C2 . H21 . 109.7 no
H22 . C2 . H21 . 110.3 no
C2 . O3 . C4 . 114.58(17) yes
O3 . C4 . C5 . 120.4(2) yes
O3 . C4 . C9 . 119.9(2) yes
C5 . C4 . C9 . 119.7(2) yes
C4 . C5 . C6 . 119.9(2) yes
C4 . C5 . H51 . 119.5 no
C6 . C5 . H51 . 120.5 no
C5 . C6 . C7 . 120.9(2) yes
C5 . C6 . H61 . 119.9 no
C7 . C6 . H61 . 119.2 no
C6 . C7 . C8 . 118.4(2) yes
C6 . C7 . C10 . 121.9(2) yes
C8 . C7 . C10 . 119.5(2) yes
C7 . C8 . C9 . 120.9(2) yes
C7 . C8 . H81 . 118.4 no
C9 . C8 . H81 . 120.7 no
C4 . C9 . C8 . 119.9(2) yes
C4 . C9 . H91 . 120.8 no
C8 . C9 . H91 . 119.3 no
C7 . C10 . N11 . 110.71(18) yes
C7 . C10 . H101 . 109.5 no
N11 . C10 . H101 . 108.1 no
C7 . C10 . H102 . 109.9 no
N11 . C10 . H102 . 108.9 no
H101 . C10 . H102 . 109.6 no
C10 . N11 . C12 . 116.8(2) yes
C10 . N11 . Pd1 . 128.34(15) yes
C12 . N11 . Pd1 . 114.48(15) yes
N11 . C12 . O13 . 128.0(2) yes
N11 . C12 . C14 . 112.8(2) yes
O13 . C12 . C14 . 119.2(2) yes
C12 . C14 . C15 . 126.8(2) yes
C12 . C14 . N19 . 113.8(2) yes
C15 . C14 . N19 . 119.4(2) yes
C12 . C14 . Pd1 . 76.64(13) yes
C15 . C14 . Pd1 . 156.25(18) yes
N19 . C14 . Pd1 . 37.29(11) yes
C14 . C15 . C16 . 118.4(2) yes
C14 . C15 . H151 . 120.4 no
C16 . C15 . H151 . 121.2 no
C15 . C16 . C17 . 121.0(2) yes
C15 . C16 . H161 . 119.5 no
C17 . C16 . H161 . 119.5 no
C16 . C17 . C18 . 117.8(2) yes
C16 . C17 . H171 . 122.1 no
C18 . C17 . H171 . 120.1 no
C17 . C18 . N19 . 119.6(2) yes
C17 . C18 . C20 . 126.3(2) yes
N19 . C18 . C20 . 114.0(2) yes
C17 . C18 . Pd1 . 156.59(18) yes
N19 . C18 . Pd1 . 37.20(11) yes
C20 . C18 . Pd1 . 76.76(13) yes
C18 . N19 . C14 . 123.7(2) yes
C18 . N19 . Pd1 . 118.11(16) yes
C14 . N19 . Pd1 . 118.01(16) yes
C18 . C20 . O21 . 120.1(2) yes
C18 . C20 . N22 . 112.68(19) yes
O21 . C20 . N22 . 127.2(2) yes
C20 . N22 . C23 . 117.05(19) yes
C20 . N22 . Pd1 . 114.81(15) yes
C23 . N22 . Pd1 . 127.39(15) yes
N22 . C23 . C24 . 110.92(19) yes
N22 . C23 . H231 . 108.2 no
C24 . C23 . H231 . 109.1 no
N22 . C23 . H232 . 109.1 no
C24 . C23 . H232 . 110.3 no
H231 . C23 . H232 . 109.2 no
C23 . C24 . C25 . 121.1(2) yes
C23 . C24 . C29 . 120.3(2) yes
C25 . C24 . C29 . 118.4(2) yes
C24 . C25 . C26 . 121.1(2) yes
C24 . C25 . H251 . 119.0 no
C26 . C25 . H251 . 119.9 no
C25 . C26 . C27 . 119.5(2) yes
C25 . C26 . H261 . 120.9 no
C27 . C26 . H261 . 119.6 no
C26 . C27 . C28 . 120.2(2) yes
C26 . C27 . O30 . 119.8(2) yes
C28 . C27 . O30 . 120.0(2) yes
C27 . C28 . C29 . 119.4(2) yes
C27 . C28 . H281 . 119.5 no
C29 . C28 . H281 . 121.1 no
C24 . C29 . C28 . 121.1(2) yes
C24 . C29 . H291 . 119.7 no
C28 . C29 . H291 . 119.2 no
C27 . O30 . C31 . 114.49(17) yes
O30 . C31 . C32 . 110.8(2) yes
O30 . C31 . H311 . 109.9 no
C32 . C31 . H311 . 111.2 no
O30 . C31 . H312 . 105.2 no
C32 . C31 . H312 . 109.3 no
H311 . C31 . H312 . 110.3 no
C31 . C32 . C1 . 127.8(2) yes
C31 . C32 . H321 . 114.6 no
C1 . C32 . H321 . 117.6 no
C34 . C33 . H332 . 108.9 no
C34 . C33 . H333 . 110.8 no
H332 . C33 . H333 . 109.3 no
C34 . C33 . H331 . 109.6 no
H332 . C33 . H331 . 109.9 no
H333 . C33 . H331 . 108.3 no
C33 . C34 . C35 . 121.7(2) yes
C33 . C34 . N39 . 117.7(2) yes
C35 . C34 . N39 . 120.7(2) yes
C34 . C35 . C36 . 119.8(2) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 120.4 no
C35 . C36 . C37 . 119.1(2) yes
C35 . C36 . H361 . 120.4 no
C37 . C36 . H361 . 120.5 no
C36 . C37 . C38 . 119.6(2) yes
C36 . C37 . H371 . 120.7 no
C38 . C37 . H371 . 119.8 no
C37 . C38 . N39 . 120.8(2) yes
C37 . C38 . C40 . 122.3(2) yes
N39 . C38 . C40 . 116.8(2) yes
C38 . N39 . C34 . 120.1(2) yes
C38 . N39 . Pd1 . 119.28(15) yes
C34 . N39 . Pd1 . 120.50(15) yes
C38 . C40 . H401 . 109.8 no
C38 . C40 . H402 . 110.3 no
H401 . C40 . H402 . 109.4 no
C38 . C40 . H403 . 110.8 no
H401 . C40 . H403 . 108.2 no
H402 . C40 . H403 . 108.3 no
C42 . C41 . C45 . 103.5(2) yes
C42 . C41 . H411 . 111.2 no
C45 . C41 . H411 . 109.8 no
C42 . C41 . H412 . 110.1 no
C45 . C41 . H412 . 110.2 no
H411 . C41 . H412 . 111.8 no
C41 . C42 . C43 . 104.3(3) yes
C41 . C42 . H421 . 112.0 no
C43 . C42 . H421 . 110.0 no
C41 . C42 . H422 . 110.8 no
C43 . C42 . H422 . 109.1 no
H421 . C42 . H422 . 110.5 no
C42 . C43 . O44 . 104.8(3) yes
C42 . C43 . H432 . 111.4 no
O44 . C43 . H432 . 110.3 no
C42 . C43 . H431 . 109.2 no
O44 . C43 . H431 . 110.1 no
H432 . C43 . H431 . 110.8 no
C43 . O44 . C45 . 109.4(2) yes
C41 . C45 . O44 . 106.0(2) yes
C41 . C45 . H452 . 111.3 no
O44 . C45 . H452 . 109.0 no
C41 . C45 . H451 . 109.4 no
O44 . C45 . H451 . 109.7 no
H452 . C45 . H451 . 111.3 no
N39 . Pd1 . N11 . 100.96(8) yes
N39 . Pd1 . N22 . 98.05(8) yes
N11 . Pd1 . N22 . 160.96(8) yes
N39 . Pd1 . N19 . 178.26(8) yes
N11 . Pd1 . N19 . 80.57(8) yes
N22 . Pd1 . N19 . 80.43(8) yes
N39 . Pd1 . C14 . 156.75(7) yes
N11 . Pd1 . C14 . 55.99(7) yes
N22 . Pd1 . C14 . 105.07(8) yes
N19 . Pd1 . C14 . 24.69(7) yes
N39 . Pd1 . C18 . 153.77(7) yes
N11 . Pd1 . C18 . 105.26(8) yes
N22 . Pd1 . C18 . 55.75(7) yes
N19 . Pd1 . C18 . 24.69(7) yes
C14 . Pd1 . C18 . 49.35(7) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C2 . H22 . O13 3_554 137.29(15) 0.964 2.339 3.117(4) yes
C2 . H21 . O44 . 177.49(15) 0.960 2.589 3.548(4) yes
C28 . H281 . O21 2_666 170.31(15) 0.933 2.421 3.344(4) yes
C17 . H171 . O30 2_666 152.83(16) 0.927 2.494 3.345(4) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 26/03/18 at 10:53:46
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 26/03/18 at 10:53:47
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
8 0 2 x .
-19 1 1 x .
-2 3 16 x .
4 4 14 x .
3 10 14 x .
_chemical_name_systematic        3-lut
####################################################################### 
# 
# 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_3-lut-dimer
_database_code_depnum_ccdc_archive 'CCDC 1879935'
_audit_update_record             
;
2018-11-20 deposited with the CCDC.
2019-01-07 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
Refinement proceded smoothly. It was possible to model the disorder present on the tetrahydrofurane 
and the chloroform molecules and it was necessary to add restriction in the bond lengths for one of
the chloroform molecule.
;
_cell_length_a                   11.9782(10)
_cell_length_b                   15.6397(12)
_cell_length_c                   21.9976(17)
_cell_angle_alpha                90
_cell_angle_beta                 94.145(4)
_cell_angle_gamma                90
_cell_volume                     4110.2(6)

_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,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

_chemical_formula_sum            'C38.83 H41.42 Cl5.17 N4 O5.28 Pd1'
_chemical_formula_moiety         
'C32 H30 N4 O4 Pd1, 1.722(C1 H1 Cl3), 1.28(C4 H8 O1)'
_chemical_compound_source        synthesized
_chemical_formula_weight         938.19


_cell_measurement_reflns_used    9870
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.46
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.48
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_max          0.64

_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1913.852
_exptl_absorpt_coefficient_mu    0.835

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex3, (Bruker, 2016)'
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  1.00
_diffrn_measurement_device_type  'Bruker Apex X8'
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

_computing_data_collection       'Apex3, (Bruker, 2016)'
_computing_cell_refinement       'Apex3, (Bruker, 2016)'
_computing_data_reduction        'Apex3, (Bruker, 2016)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0

_diffrn_ambient_temperature      100
_diffrn_reflns_number            87723
_reflns_number_total             9433
_diffrn_reflns_av_R_equivalents  0.037

_diffrn_reflns_theta_min         1.599
_diffrn_reflns_theta_max         27.494
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        27.494
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   1.64
_oxford_diffrn_Wilson_scale      334.71

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.57
_refine_diff_density_max         1.90


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         9395
_refine_ls_number_restraints     3
_refine_ls_number_parameters     595
_oxford_refine_ls_R_factor_ref   0.0486
_refine_ls_wR_factor_ref         0.1001
_refine_ls_goodness_of_fit_ref   0.9316
_refine_ls_shift/su_max          0.0013703
_refine_ls_shift/su_mean         0.0000391


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9397
_refine_ls_R_factor_all          0.0486
_refine_ls_wR_factor_all         0.1001

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8181
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_gt          0.0952

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 4.62 6.81 3.11 0.790 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 1.1473(2) 0.28967(19) 0.04219(13) 0.0274 1.0000 Uani . . . . . .
C2 C 1.1064(3) 0.2790(2) 0.10406(14) 0.0324 1.0000 Uani . . . . . .
O3 O 0.99426(19) 0.24666(15) 0.09865(9) 0.0338 1.0000 Uani . . . . . .
C4 C 0.9375(2) 0.24247(18) 0.15075(13) 0.0268 1.0000 Uani . . . . . .
C5 C 0.9824(2) 0.26210(19) 0.20877(13) 0.0272 1.0000 Uani . . . . . .
C6 C 0.9148(2) 0.25758(18) 0.25788(12) 0.0248 1.0000 Uani . . . . . .
C7 C 0.8030(2) 0.23283(17) 0.25013(12) 0.0222 1.0000 Uani . . . . . .
C8 C 0.7601(2) 0.21241(19) 0.19157(13) 0.0266 1.0000 Uani . . . . . .
C9 C 0.8256(3) 0.2168(2) 0.14194(13) 0.0306 1.0000 Uani . . . . . .
C10 C 0.7298(2) 0.22997(17) 0.30363(12) 0.0222 1.0000 Uani . . . . . .
N11 N 0.73956(18) 0.30761(14) 0.34080(10) 0.0205 1.0000 Uani . . . . . .
C12 C 0.8027(2) 0.30337(18) 0.39383(12) 0.0234 1.0000 Uani . . . . . .
O13 O 0.85373(19) 0.24023(14) 0.41572(10) 0.0325 1.0000 Uani . . . . . .
C14 C 0.8082(2) 0.38777(18) 0.42763(11) 0.0216 1.0000 Uani . . . . . .
C15 C 0.8659(2) 0.4052(2) 0.48307(13) 0.0269 1.0000 Uani . . . . . .
C16 C 0.8623(2) 0.4876(2) 0.50626(13) 0.0285 1.0000 Uani . . . . . .
C17 C 0.8008(2) 0.55155(19) 0.47465(12) 0.0244 1.0000 Uani . . . . . .
C18 C 0.7437(2) 0.53044(17) 0.41961(11) 0.0209 1.0000 Uani . . . . . .
N19 N 0.74980(18) 0.45037(14) 0.39870(9) 0.0191 1.0000 Uani . . . . . .
C20 C 0.6724(2) 0.58890(17) 0.37850(11) 0.0200 1.0000 Uani . . . . . .
O21 O 0.66100(17) 0.66548(12) 0.39239(9) 0.0248 1.0000 Uani . . . . . .
N22 N 0.62711(18) 0.54852(14) 0.32845(10) 0.0197 1.0000 Uani . . . . . .
C23 C 0.5549(2) 0.59852(17) 0.28579(11) 0.0202 1.0000 Uani . . . . . .
C24 C 0.6121(2) 0.62321(16) 0.22880(11) 0.0207 1.0000 Uani . . . . . .
C25 C 0.7218(2) 0.65404(17) 0.23269(12) 0.0229 1.0000 Uani . . . . . .
C26 C 0.7767(2) 0.67569(19) 0.18075(13) 0.0254 1.0000 Uani . . . . . .
C27 C 0.7206(2) 0.66662(19) 0.12364(12) 0.0262 1.0000 Uani . . . . . .
C28 C 0.6103(2) 0.6364(2) 0.11902(13) 0.0298 1.0000 Uani . . . . . .
C29 C 0.5576(2) 0.61476(19) 0.17106(13) 0.0256 1.0000 Uani . . . . . .
O30 O 0.76564(17) 0.68454(16) 0.06958(9) 0.0329 1.0000 Uani . . . . . .
C31 C 0.8826(2) 0.7035(2) 0.07161(13) 0.0294 1.0000 Uani . . . . . .
C32 C 0.9182(3) 0.7130(2) 0.00863(14) 0.0312 1.0000 Uani . . . . . .
C33 C 0.7542(2) 0.43903(18) 0.18637(12) 0.0257 1.0000 Uani . . . . . .
C34 C 0.6372(2) 0.40541(17) 0.18477(12) 0.0233 1.0000 Uani . . . . . .
C35 C 0.5792(3) 0.3835(2) 0.12960(13) 0.0321 1.0000 Uani . . . . . .
C36 C 0.4731(3) 0.3498(2) 0.12978(15) 0.0376 1.0000 Uani . . . . . .
C37 C 0.4245(3) 0.3386(2) 0.18453(16) 0.0338 1.0000 Uani . . . . . .
C38 C 0.4838(2) 0.36210(17) 0.23836(14) 0.0258 1.0000 Uani . . . . . .
N39 N 0.58864(18) 0.39443(14) 0.23802(10) 0.0202 1.0000 Uani . . . . . .
C40 C 0.4358(2) 0.3521(2) 0.29900(15) 0.0308 1.0000 Uani . . . . . .
C41 C 1.0497(5) 0.5056(4) 0.2575(3) 0.0418 0.7851 Uani . . . . 1 .
C42 C 1.1679(5) 0.4710(5) 0.2718(3) 0.0552 0.7851 Uani . . . . 1 .
C43 C 1.1657(10) 0.4367(9) 0.3381(4) 0.0769 0.7851 Uani . . . . 1 .
O44 O 1.0560(3) 0.4342(2) 0.35291(15) 0.0463 0.7851 Uani . . . . 1 .
C45 C 0.9950(7) 0.4944(7) 0.3164(5) 0.0544 0.7851 Uani . . . . 1 .
C46 C 0.7253(9) 0.4804(6) -0.0812(4) 0.0567 0.4932 Uani . . . . 6 .
C47 C 0.8452(8) 0.4637(6) -0.0530(4) 0.0483 0.4932 Uani . . . . 6 .
C48 C 0.8337(10) 0.4304(6) 0.0174(6) 0.0590 0.4932 Uani . . . . 6 .
C49 C 0.6629(12) 0.4944(10) -0.0262(6) 0.0476 0.4932 Uani . . . . 6 .
O50 O 0.7166(8) 0.4528(5) 0.0226(4) 0.0874 0.4932 Uani . . . . 6 .
C51 C 1.0770(17) 0.5276(17) 0.2828(10) 0.0518 0.2149 Uani D . . . 2 .
C52 C 0.7934(9) 0.4379(5) -0.0434(3) 0.0438 0.5068 Uani . . . . 5 .
C53 C 0.5185(4) 0.1703(3) 0.01712(18) 0.0482 1.0000 Uani . . . . . .
Pd1 Pd 0.672296(15) 0.424007(12) 0.320580(8) 0.0167 1.0000 Uani . . . . . .
Cl42 Cl 0.60896(17) 0.25461(11) -0.00341(8) 0.0253 0.5276 Uani . . . . 3 .
Cl43 Cl 0.4713(3) 0.1083(2) -0.04367(16) 0.0760 0.5276 Uani . . . . 3 .
Cl44 Cl 0.5947(3) 0.09152(18) 0.0601(2) 0.0632 0.5276 Uani . . . . 3 .
Cl1 Cl 0.8610(2) 0.4637(2) 0.02654(12) 0.0569 0.5068 Uani . . . . 5 .
Cl2 Cl 0.8636(3) 0.48485(15) -0.10244(12) 0.0952 0.5068 Uani . . . . 5 .
Cl3 Cl 0.6532(4) 0.4732(3) -0.0462(2) 0.0793 0.5068 Uani . . . . 5 .
Cl6 Cl 1.0486(9) 0.5161(5) 0.2063(4) 0.1034 0.2149 Uani D . . . 2 .
Cl15 Cl 0.9616(7) 0.5117(6) 0.3230(5) 0.0607 0.2149 Uani D . . . 2 .
Cl18 Cl 1.1846(10) 0.4639(12) 0.3150(9) 0.1463 0.2149 Uani D . . . 2 .
Cl5 Cl 0.4314(3) 0.1435(2) -0.05009(16) 0.0631 0.4724 Uani . . . . 4 .
Cl4 Cl 0.5937(8) 0.0983(6) 0.0540(6) 0.1653 0.4724 Uani . . . . 4 .
Cl14 Cl 0.6074(7) 0.2434(5) -0.0017(4) 0.1670 0.4724 Uani . . . . 4 .
H331 H 0.7682 0.4628 0.1484 0.0391 1.0000 Uiso R . . . . .
H333 H 0.7647 0.4827 0.2157 0.0385 1.0000 Uiso R . . . . .
H332 H 0.8051 0.3959 0.1953 0.0393 1.0000 Uiso R . . . . .
H351 H 0.6126 0.3927 0.0933 0.0384 1.0000 Uiso R . . . . .
H361 H 0.4344 0.3354 0.0932 0.0438 1.0000 Uiso R . . . . .
H371 H 0.3532 0.3154 0.1855 0.0398 1.0000 Uiso R . . . . .
H401 H 0.3619 0.3284 0.2939 0.0456 1.0000 Uiso R . . . . .
H403 H 0.4309 0.4075 0.3181 0.0457 1.0000 Uiso R . . . . .
H402 H 0.4834 0.3165 0.3254 0.0465 1.0000 Uiso R . . . . .
H231 H 0.5348 0.6509 0.3062 0.0252 1.0000 Uiso R . . . . .
H232 H 0.4880 0.5646 0.2740 0.0250 1.0000 Uiso R . . . . .
H291 H 0.4838 0.5921 0.1670 0.0298 1.0000 Uiso R . . . . .
H281 H 0.5712 0.6303 0.0814 0.0360 1.0000 Uiso R . . . . .
H312 H 0.8985 0.7573 0.0939 0.0384 1.0000 Uiso R . . . . .
H311 H 0.9255 0.6570 0.0937 0.0378 1.0000 Uiso R . . . . .
H321 H 0.9960 0.7221 0.0057 0.0368 1.0000 Uiso R . . . . .
H11 H 1.2240 0.2977 0.0395 0.0326 1.0000 Uiso R . . . . .
H22 H 1.1537 0.2375 0.1281 0.0405 1.0000 Uiso R . . . . .
H21 H 1.1081 0.3349 0.1250 0.0402 1.0000 Uiso R . . . . .
H51 H 1.0578 0.2783 0.2149 0.0323 1.0000 Uiso R . . . . .
H61 H 0.9459 0.2729 0.2967 0.0286 1.0000 Uiso R . . . . .
H101 H 0.7522 0.1817 0.3292 0.0268 1.0000 Uiso R . . . . .
H102 H 0.6509 0.2230 0.2883 0.0268 1.0000 Uiso R . . . . .
H151 H 0.9052 0.3610 0.5037 0.0322 1.0000 Uiso R . . . . .
H161 H 0.9022 0.5005 0.5430 0.0344 1.0000 Uiso R . . . . .
H171 H 0.7982 0.6080 0.4891 0.0294 1.0000 Uiso R . . . . .
H81 H 0.6849 0.1961 0.1850 0.0317 1.0000 Uiso R . . . . .
H91 H 0.7941 0.2033 0.1030 0.0367 1.0000 Uiso R . . . . .
H261 H 0.8510 0.6950 0.1841 0.0296 1.0000 Uiso R . . . . .
H251 H 0.7608 0.6597 0.2713 0.0282 1.0000 Uiso R . . . . .
H521 H 0.7934 0.3760 -0.0487 0.0481 0.5068 Uiso R . . . 5 .
H452 H 0.9969 0.5491 0.3380 0.0541 0.7851 Uiso R . . . 1 .
H451 H 0.9192 0.4725 0.3083 0.0540 0.7851 Uiso R . . . 1 .
H411 H 1.0486 0.5659 0.2458 0.0511 0.7851 Uiso R . . . 1 .
H412 H 1.0087 0.4700 0.2267 0.0515 0.7851 Uiso R . . . 1 .
H421 H 1.2232 0.5148 0.2674 0.0664 0.7851 Uiso R . . . 1 .
H422 H 1.1803 0.4245 0.2450 0.0666 0.7851 Uiso R . . . 1 .
H432 H 1.2054 0.4775 0.3652 0.0897 0.7851 Uiso R . . . 1 .
H431 H 1.1976 0.3813 0.3436 0.0894 0.7851 Uiso R . . . 1 .
H511 H 1.1004 0.5871 0.2889 0.0651 0.2149 Uiso R . . . 2 .
H462 H 0.7263 0.5289 -0.1075 0.0662 0.4932 Uiso R . . . 6 .
H461 H 0.6986 0.4317 -0.1038 0.0662 0.4932 Uiso R . . . 6 .
H471 H 0.8928 0.5142 -0.0543 0.0610 0.4932 Uiso R . . . 6 .
H472 H 0.8804 0.4195 -0.0765 0.0611 0.4932 Uiso R . . . 6 .
H482 H 0.8844 0.4598 0.0460 0.0654 0.4932 Uiso R . . . 6 .
H481 H 0.8435 0.3697 0.0207 0.0652 0.4932 Uiso R . . . 6 .
H492 H 0.6586 0.5546 -0.0175 0.0559 0.4932 Uiso R . . . 6 .
H491 H 0.5879 0.4719 -0.0327 0.0563 0.4932 Uiso R . . . 6 .
H531 H 0.4719 0.1956 0.0453 0.0614 0.4724 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.073061(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C32 2_765 1.319(4) yes
C1 . C2 . 1.489(4) yes
C1 . H11 . 0.932 no
C2 . O3 . 1.432(4) yes
C2 . H22 . 0.989 no
C2 . H21 . 0.987 no
O3 . C4 . 1.376(3) yes
C4 . C5 . 1.383(4) yes
C4 . C9 . 1.400(4) yes
C5 . C6 . 1.398(4) yes
C5 . H51 . 0.938 no
C6 . C7 . 1.392(4) yes
C6 . H61 . 0.938 no
C7 . C8 . 1.389(4) yes
C7 . C10 . 1.519(3) yes
C8 . C9 . 1.391(4) yes
C8 . H81 . 0.937 no
C9 . H91 . 0.935 no
C10 . N11 . 1.464(3) yes
C10 . H101 . 0.969 no
C10 . H102 . 0.986 no
N11 . C12 . 1.346(3) yes
N11 . Pd1 . 2.027(2) yes
C12 . O13 . 1.240(3) yes
C12 . C14 . 1.514(4) yes
C14 . C15 . 1.385(4) yes
C14 . N19 . 1.338(3) yes
C14 . Pd1 . 2.822(3) yes
C15 . C16 . 1.389(4) yes
C15 . H151 . 0.934 no
C16 . C17 . 1.397(4) yes
C16 . H161 . 0.931 no
C17 . C18 . 1.387(4) yes
C17 . H171 . 0.939 no
C18 . N19 . 1.338(3) yes
C18 . C20 . 1.507(4) yes
C18 . Pd1 . 2.825(3) yes
N19 . Pd1 . 1.938(2) yes
C20 . O21 . 1.246(3) yes
C20 . N22 . 1.349(3) yes
N22 . C23 . 1.457(3) yes
N22 . Pd1 . 2.032(2) yes
C23 . C24 . 1.521(3) yes
C23 . H231 . 0.973 no
C23 . H232 . 0.980 no
C24 . C25 . 1.397(4) yes
C24 . C29 . 1.392(4) yes
C25 . C26 . 1.400(4) yes
C25 . H251 . 0.943 no
C26 . C27 . 1.389(4) yes
C26 . H261 . 0.937 no
C27 . C28 . 1.400(4) yes
C27 . O30 . 1.370(3) yes
C28 . C29 . 1.388(4) yes
C28 . H281 . 0.925 no
C29 . H291 . 0.951 no
O30 . C31 . 1.429(3) yes
C31 . C32 . 1.486(4) yes
C31 . H312 . 0.985 no
C31 . H311 . 0.997 no
C32 . H321 . 0.950 no
C33 . C34 . 1.495(4) yes
C33 . H331 . 0.940 no
C33 . H333 . 0.941 no
C33 . H332 . 0.921 no
C34 . C35 . 1.397(4) yes
C34 . N39 . 1.356(3) yes
C35 . C36 . 1.377(5) yes
C35 . H351 . 0.931 no
C36 . C37 . 1.386(5) yes
C36 . H361 . 0.928 no
C37 . C38 . 1.386(4) yes
C37 . H371 . 0.930 no
C38 . N39 . 1.354(3) yes
C38 . C40 . 1.499(4) yes
N39 . Pd1 . 2.062(2) yes
C40 . H401 . 0.958 no
C40 . H403 . 0.967 no
C40 . H402 . 0.961 no
C41 . C42 . 1.528(9) yes
C41 . C45 . 1.504(10) yes
C41 . H411 . 0.977 no
C41 . H412 . 0.980 no
C42 . C43 . 1.556(11) yes
C42 . H421 . 0.963 no
C42 . H422 . 0.953 no
C43 . O44 . 1.377(11) yes
C43 . H432 . 0.973 no
C43 . H431 . 0.951 no
O44 . C45 . 1.408(11) yes
C45 . H452 . 0.976 no
C45 . H451 . 0.974 no
C46 . C47 . 1.545(13) yes
C46 . C49 . 1.485(15) yes
C46 . H462 . 0.954 no
C46 . H461 . 0.952 no
C47 . C48 . 1.649(17) yes
C47 . H471 . 0.975 no
C47 . H472 . 0.976 no
C48 . O50 . 1.459(14) yes
C48 . H482 . 0.960 no
C48 . H481 . 0.958 no
C49 . O50 . 1.374(16) yes
C49 . H492 . 0.963 no
C49 . H491 . 0.965 no
C51 . Cl6 . 1.70(2) yes
C51 . Cl15 . 1.71(2) yes
C51 . Cl18 . 1.74(2) yes
C51 . H511 . 0.979 no
C52 . Cl1 . 1.734(8) yes
C52 . Cl2 . 1.757(8) yes
C52 . Cl3 . 1.765(11) yes
C52 . H521 . 0.975 no
C53 . Cl42 . 1.785(5) yes
C53 . Cl43 . 1.715(5) yes
C53 . Cl44 . 1.767(5) yes
C53 . H531 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C32 2_765 C1 . C2 . 123.8(3) yes
C32 2_765 C1 . H11 . 118.5 no
C2 . C1 . H11 . 117.7 no
C1 . C2 . O3 . 109.4(2) yes
C1 . C2 . H22 . 110.4 no
O3 . C2 . H22 . 108.1 no
C1 . C2 . H21 . 109.2 no
O3 . C2 . H21 . 109.8 no
H22 . C2 . H21 . 109.9 no
C2 . O3 . C4 . 117.7(2) yes
O3 . C4 . C5 . 125.1(3) yes
O3 . C4 . C9 . 115.1(3) yes
C5 . C4 . C9 . 119.8(3) yes
C4 . C5 . C6 . 119.6(3) yes
C4 . C5 . H51 . 119.9 no
C6 . C5 . H51 . 120.5 no
C5 . C6 . C7 . 121.7(3) yes
C5 . C6 . H61 . 118.4 no
C7 . C6 . H61 . 119.9 no
C6 . C7 . C8 . 117.8(2) yes
C6 . C7 . C10 . 121.2(2) yes
C8 . C7 . C10 . 121.0(2) yes
C7 . C8 . C9 . 121.6(3) yes
C7 . C8 . H81 . 119.5 no
C9 . C8 . H81 . 118.9 no
C4 . C9 . C8 . 119.6(3) yes
C4 . C9 . H91 . 120.7 no
C8 . C9 . H91 . 119.6 no
C7 . C10 . N11 . 112.4(2) yes
C7 . C10 . H101 . 108.8 no
N11 . C10 . H101 . 108.3 no
C7 . C10 . H102 . 109.4 no
N11 . C10 . H102 . 108.6 no
H101 . C10 . H102 . 109.3 no
C10 . N11 . C12 . 117.4(2) yes
C10 . N11 . Pd1 . 127.43(17) yes
C12 . N11 . Pd1 . 115.10(18) yes
N11 . C12 . O13 . 127.3(3) yes
N11 . C12 . C14 . 112.6(2) yes
O13 . C12 . C14 . 120.1(2) yes
C12 . C14 . C15 . 127.2(3) yes
C12 . C14 . N19 . 113.7(2) yes
C15 . C14 . N19 . 119.1(3) yes
C12 . C14 . Pd1 . 76.32(14) yes
C15 . C14 . Pd1 . 156.4(2) yes
N19 . C14 . Pd1 . 37.39(12) yes
C14 . C15 . C16 . 118.7(3) yes
C14 . C15 . H151 . 118.9 no
C16 . C15 . H151 . 122.4 no
C15 . C16 . C17 . 120.7(3) yes
C15 . C16 . H161 . 119.5 no
C17 . C16 . H161 . 119.8 no
C16 . C17 . C18 . 118.3(3) yes
C16 . C17 . H171 . 122.2 no
C18 . C17 . H171 . 119.5 no
C17 . C18 . N19 . 119.1(3) yes
C17 . C18 . C20 . 127.0(2) yes
N19 . C18 . C20 . 113.9(2) yes
C17 . C18 . Pd1 . 156.4(2) yes
N19 . C18 . Pd1 . 37.28(12) yes
C20 . C18 . Pd1 . 76.58(14) yes
C18 . N19 . C14 . 124.2(2) yes
C18 . N19 . Pd1 . 117.99(18) yes
C14 . N19 . Pd1 . 117.83(18) yes
C18 . C20 . O21 . 120.2(2) yes
C18 . C20 . N22 . 112.5(2) yes
O21 . C20 . N22 . 127.3(2) yes
C20 . N22 . C23 . 117.4(2) yes
C20 . N22 . Pd1 . 115.11(17) yes
C23 . N22 . Pd1 . 127.51(17) yes
N22 . C23 . C24 . 112.7(2) yes
N22 . C23 . H231 . 108.1 no
C24 . C23 . H231 . 107.9 no
N22 . C23 . H232 . 108.4 no
C24 . C23 . H232 . 109.1 no
H231 . C23 . H232 . 110.7 no
C23 . C24 . C25 . 121.0(2) yes
C23 . C24 . C29 . 121.2(2) yes
C25 . C24 . C29 . 117.8(2) yes
C24 . C25 . C26 . 121.9(2) yes
C24 . C25 . H251 . 119.4 no
C26 . C25 . H251 . 118.7 no
C25 . C26 . C27 . 119.2(3) yes
C25 . C26 . H261 . 120.9 no
C27 . C26 . H261 . 119.9 no
C26 . C27 . C28 . 119.5(2) yes
C26 . C27 . O30 . 124.7(3) yes
C28 . C27 . O30 . 115.8(2) yes
C27 . C28 . C29 . 120.3(3) yes
C27 . C28 . H281 . 120.9 no
C29 . C28 . H281 . 118.8 no
C24 . C29 . C28 . 121.2(3) yes
C24 . C29 . H291 . 119.5 no
C28 . C29 . H291 . 119.3 no
C27 . O30 . C31 . 117.5(2) yes
O30 . C31 . C32 . 109.8(2) yes
O30 . C31 . H312 . 110.3 no
C32 . C31 . H312 . 108.7 no
O30 . C31 . H311 . 109.5 no
C32 . C31 . H311 . 110.8 no
H312 . C31 . H311 . 107.8 no
C31 . C32 . C1 2_765 126.4(3) yes
C31 . C32 . H321 . 115.3 no
C1 2_765 C32 . H321 . 118.2 no
C34 . C33 . H331 . 110.2 no
C34 . C33 . H333 . 110.5 no
H331 . C33 . H333 . 107.3 no
C34 . C33 . H332 . 110.6 no
H331 . C33 . H332 . 108.7 no
H333 . C33 . H332 . 109.4 no
C33 . C34 . C35 . 120.9(3) yes
C33 . C34 . N39 . 118.9(2) yes
C35 . C34 . N39 . 120.2(3) yes
C34 . C35 . C36 . 119.5(3) yes
C34 . C35 . H351 . 119.4 no
C36 . C35 . H351 . 121.0 no
C35 . C36 . C37 . 119.8(3) yes
C35 . C36 . H361 . 119.6 no
C37 . C36 . H361 . 120.6 no
C36 . C37 . C38 . 119.2(3) yes
C36 . C37 . H371 . 120.9 no
C38 . C37 . H371 . 119.9 no
C37 . C38 . N39 . 120.9(3) yes
C37 . C38 . C40 . 121.8(3) yes
N39 . C38 . C40 . 117.4(2) yes
C34 . N39 . C38 . 120.5(2) yes
C34 . N39 . Pd1 . 121.41(18) yes
C38 . N39 . Pd1 . 118.08(18) yes
C38 . C40 . H401 . 110.3 no
C38 . C40 . H403 . 109.4 no
H401 . C40 . H403 . 108.2 no
C38 . C40 . H402 . 110.4 no
H401 . C40 . H402 . 110.5 no
H403 . C40 . H402 . 108.0 no
C42 . C41 . C45 . 103.7(6) yes
C42 . C41 . H411 . 113.0 no
C45 . C41 . H411 . 109.9 no
C42 . C41 . H412 . 110.6 no
C45 . C41 . H412 . 107.6 no
H411 . C41 . H412 . 111.7 no
C41 . C42 . C43 . 103.7(6) yes
C41 . C42 . H421 . 111.2 no
C43 . C42 . H421 . 113.5 no
C41 . C42 . H422 . 109.0 no
C43 . C42 . H422 . 109.2 no
H421 . C42 . H422 . 110.0 no
C42 . C43 . O44 . 108.2(8) yes
C42 . C43 . H432 . 107.9 no
O44 . C43 . H432 . 107.8 no
C42 . C43 . H431 . 113.6 no
O44 . C43 . H431 . 109.0 no
H432 . C43 . H431 . 110.2 no
C43 . O44 . C45 . 108.1(6) yes
C41 . C45 . O44 . 109.2(5) yes
C41 . C45 . H452 . 108.7 no
O44 . C45 . H452 . 108.4 no
C41 . C45 . H451 . 110.0 no
O44 . C45 . H451 . 107.9 no
H452 . C45 . H451 . 112.7 no
C47 . C46 . C49 . 101.9(8) yes
C47 . C46 . H462 . 109.0 no
C49 . C46 . H462 . 114.0 no
C47 . C46 . H461 . 110.0 no
C49 . C46 . H461 . 111.9 no
H462 . C46 . H461 . 109.8 no
C46 . C47 . C48 . 107.0(9) yes
C46 . C47 . H471 . 112.4 no
C48 . C47 . H471 . 111.8 no
C46 . C47 . H472 . 109.4 no
C48 . C47 . H472 . 109.9 no
H471 . C47 . H472 . 106.4 no
C47 . C48 . O50 . 98.3(9) yes
C47 . C48 . H482 . 111.9 no
O50 . C48 . H482 . 113.5 no
C47 . C48 . H481 . 111.5 no
O50 . C48 . H481 . 110.2 no
H482 . C48 . H481 . 110.9 no
C46 . C49 . O50 . 109.4(11) yes
C46 . C49 . H492 . 110.1 no
O50 . C49 . H492 . 109.7 no
C46 . C49 . H491 . 110.1 no
O50 . C49 . H491 . 108.7 no
H492 . C49 . H491 . 108.8 no
C48 . O50 . C49 . 116.8(9) yes
Cl6 . C51 . Cl15 . 112.6(13) yes
Cl6 . C51 . Cl18 . 115.6(15) yes
Cl15 . C51 . Cl18 . 108.0(14) yes
Cl6 . C51 . H511 . 105.7 no
Cl15 . C51 . H511 . 107.5 no
Cl18 . C51 . H511 . 107.0 no
Cl1 . C52 . Cl2 . 109.9(5) yes
Cl1 . C52 . Cl3 . 109.9(5) yes
Cl2 . C52 . Cl3 . 110.4(5) yes
Cl1 . C52 . H521 . 109.4 no
Cl2 . C52 . H521 . 108.9 no
Cl3 . C52 . H521 . 108.3 no
Cl42 . C53 . Cl43 . 113.1(3) yes
Cl42 . C53 . Cl44 . 110.5(3) yes
Cl43 . C53 . Cl44 . 98.7(3) yes
Cl42 . C53 . H531 . 104.7 no
Cl43 . C53 . H531 . 124.7 no
Cl44 . C53 . H531 . 104.2 no
N39 . Pd1 . N22 . 100.05(9) yes
N39 . Pd1 . N11 . 98.73(9) yes
N22 . Pd1 . N11 . 161.10(9) yes
N39 . Pd1 . N19 . 179.14(9) yes
N22 . Pd1 . N19 . 80.44(9) yes
N11 . Pd1 . N19 . 80.74(9) yes
N39 . Pd1 . C14 . 154.70(8) yes
N22 . Pd1 . C14 . 105.22(8) yes
N11 . Pd1 . C14 . 55.97(9) yes
N19 . Pd1 . C14 . 24.78(9) yes
N39 . Pd1 . C18 . 155.79(8) yes
N22 . Pd1 . C18 . 55.74(8) yes
N11 . Pd1 . C18 . 105.47(8) yes
N19 . Pd1 . C18 . 24.72(9) yes
C14 . Pd1 . C18 . 49.50(8) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C35 . H351 . O50 . 161.0(3) 0.931 2.265 3.159(7) yes
C32 . H321 . O13 4_755 130.63(9) 0.950 2.421 3.124(7) yes
C2 . H22 . O21 4_745 131.71(8) 0.989 2.559 3.300(7) yes
C16 . H161 . O44 2_766 158.57(11) 0.931 2.524 3.407(7) yes
C52 . H521 . O13 3_554 153.5(2) 0.975 2.127 3.031(7) yes
C51 . H511 . C8 4_755 156.5(5) 0.979 2.591 3.511(7) yes
C47 . H472 . O13 3_554 132.8(2) 0.976 2.523 3.266(7) yes
C53 . H531 . O21 4_645 142.59(12) 0.950 2.224 3.034(7) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 26/03/18 at 10:52:20
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  31,X'S) H   ( 312,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 333,X'S) H   ( 332,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 403,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) 
RIDE C   (  45,X'S) H   ( 452,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 462,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 492,X'S) H   ( 491,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 26/03/18 at 10:52:21
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.780000 , 0.050000 = CL(18) TO C(51) 
DISTANCE 1.780000 , 0.050000 = CL(15) TO C(51) 
DISTANCE 1.780000 , 0.050000 = CL(6) TO C(51) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
3 6 23 x .
3 0 4 x .
