# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_cu_8v00201_0m
_database_code_depnum_ccdc_archive 'CCDC 2060195'
loop_
_audit_author_name
_audit_author_address
'Georgina M. Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2020-10-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H56 N2 O4 Pd'
_chemical_formula_sum            'C39 H56 N2 O4 Pd'
_chemical_formula_weight         723.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   23.5009(5)
_cell_length_b                   5.88070(10)
_cell_length_c                   28.0066(6)
_cell_angle_alpha                90
_cell_angle_beta                 106.1280(10)
_cell_angle_gamma                90
_cell_volume                     3718.23(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      74.769
_cell_measurement_theta_min      5.774
_shelx_estimated_absorpt_T_max   0.846
_shelx_estimated_absorpt_T_min   0.290
_exptl_absorpt_coefficient_mu    4.336
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1209 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.6408.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            81773
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.842
_diffrn_reflns_theta_min         3.285
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7201
_reflns_number_total             7626
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0217
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0294P)²+2.0953P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0576
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C23(H23A,H23B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C16(H16), C18(H18), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.68720(2) 0.49791(2) 0.38754(2) 0.01128(4) Uani 1 1 d . . . . .
O1 O 0.69356(4) 0.42343(17) 0.31952(3) 0.01392(18) Uani 1 1 d . . . . .
O2 O 0.66922(4) 0.5664(2) 0.45123(4) 0.0208(2) Uani 1 1 d . . . . .
O3 O 0.90054(4) 0.62180(18) 0.46385(4) 0.0225(2) Uani 1 1 d . . . . .
O4 O 0.89092(4) 0.29879(17) 0.50406(4) 0.0210(2) Uani 1 1 d . . . . .
N1 N 0.77310(5) 0.60537(18) 0.41342(4) 0.0121(2) Uani 1 1 d . . . . .
N2 N 0.60259(5) 0.3791(2) 0.36297(4) 0.0160(2) Uani 1 1 d . . . . .
C1 C 0.74426(5) 0.3398(2) 0.31380(4) 0.0125(2) Uani 1 1 d . . . . .
C2 C 0.74404(5) 0.1572(2) 0.28074(4) 0.0128(2) Uani 1 1 d . . . . .
C3 C 0.79878(6) 0.0778(2) 0.27699(5) 0.0145(2) Uani 1 1 d . . . . .
H3 H 0.798895 -0.044190 0.254784 0.017 Uiso 1 1 calc R U . . .
C4 C 0.85328(6) 0.1676(2) 0.30403(5) 0.0146(2) Uani 1 1 d . . . . .
C5 C 0.85193(5) 0.3512(2) 0.33518(5) 0.0145(2) Uani 1 1 d . . . . .
H5 H 0.888134 0.417833 0.353774 0.017 Uiso 1 1 calc R U . . .
C6 C 0.79869(6) 0.4388(2) 0.33957(5) 0.0133(2) Uani 1 1 d . . . . .
C7 C 0.79773(5) 0.6484(2) 0.36987(4) 0.0130(2) Uani 1 1 d . . . . .
H7A H 0.773427 0.766183 0.348261 0.016 Uiso 1 1 calc R U . . .
H7B H 0.838560 0.708141 0.382354 0.016 Uiso 1 1 calc R U . . .
C8 C 0.77224(6) 0.8251(2) 0.43996(5) 0.0137(2) Uani 1 1 d . . . . .
H8A H 0.745195 0.931164 0.416981 0.016 Uiso 1 1 calc R U . . .
H8B H 0.812452 0.892001 0.448255 0.016 Uiso 1 1 calc R U . . .
C9 C 0.75320(5) 0.8082(2) 0.48699(5) 0.0140(2) Uani 1 1 d . . . . .
C10 C 0.70059(6) 0.6958(2) 0.48841(5) 0.0149(2) Uani 1 1 d . . . . .
C11 C 0.68031(5) 0.7226(2) 0.53139(5) 0.0144(2) Uani 1 1 d . . . . .
C12 C 0.62012(6) 0.6228(2) 0.53254(5) 0.0159(3) Uani 1 1 d . . . . .
C13 C 0.62293(6) 0.3615(2) 0.53222(5) 0.0213(3) Uani 1 1 d . . . . .
H13A H 0.636389 0.310690 0.503849 0.032 Uiso 1 1 calc R U . . .
H13B H 0.583474 0.299123 0.529460 0.032 Uiso 1 1 calc R U . . .
H13C H 0.650703 0.308228 0.563147 0.032 Uiso 1 1 calc R U . . .
C14 C 0.57072(6) 0.7111(3) 0.48771(5) 0.0211(3) Uani 1 1 d . . . . .
H14A H 0.568830 0.877286 0.489193 0.032 Uiso 1 1 calc R U . . .
H14B H 0.532626 0.646391 0.488685 0.032 Uiso 1 1 calc R U . . .
H14C H 0.579344 0.665467 0.456785 0.032 Uiso 1 1 calc R U . . .
C15 C 0.60258(6) 0.6932(3) 0.57929(5) 0.0243(3) Uani 1 1 d . . . . .
H15A H 0.631531 0.632571 0.608793 0.036 Uiso 1 1 calc R U . . .
H15B H 0.563234 0.632373 0.577569 0.036 Uiso 1 1 calc R U . . .
H15C H 0.601772 0.859428 0.581347 0.036 Uiso 1 1 calc R U . . .
C16 C 0.71617(6) 0.8399(2) 0.57198(5) 0.0144(2) Uani 1 1 d . . . . .
H16 H 0.702810 0.854405 0.600891 0.017 Uiso 1 1 calc R U . . .
C17 C 0.77057(6) 0.9371(2) 0.57258(5) 0.0144(2) Uani 1 1 d . . . . .
C18 C 0.78743(6) 0.9218(2) 0.52885(5) 0.0143(2) Uani 1 1 d . . . . .
H18 H 0.823460 0.991051 0.527459 0.017 Uiso 1 1 calc R U . . .
C19 C 0.80996(6) 1.0647(3) 0.61767(5) 0.0166(3) Uani 1 1 d . . . . .
C20 C 0.78995(8) 1.0273(3) 0.66449(6) 0.0325(4) Uani 1 1 d . . . . .
H20A H 0.817496 1.103765 0.692668 0.049 Uiso 1 1 calc R U . . .
H20B H 0.789415 0.864012 0.671344 0.049 Uiso 1 1 calc R U . . .
H20C H 0.750095 1.090080 0.659496 0.049 Uiso 1 1 calc R U . . .
C21 C 0.87416(7) 0.9795(3) 0.62900(6) 0.0235(3) Uani 1 1 d . . . . .
H21A H 0.898894 1.061542 0.657790 0.035 Uiso 1 1 calc R U . . .
H21B H 0.889091 1.006371 0.600111 0.035 Uiso 1 1 calc R U . . .
H21C H 0.875417 0.816341 0.636313 0.035 Uiso 1 1 calc R U . . .
C22 C 0.80870(8) 1.3194(3) 0.60599(6) 0.0318(4) Uani 1 1 d . . . . .
H22A H 0.768029 1.376153 0.599335 0.048 Uiso 1 1 calc R U . . .
H22B H 0.822996 1.344198 0.576695 0.048 Uiso 1 1 calc R U . . .
H22C H 0.834260 1.400952 0.634463 0.048 Uiso 1 1 calc R U . . .
C23 C 0.80563(5) 0.4239(2) 0.44670(5) 0.0137(2) Uani 1 1 d . . . . .
H23A H 0.802353 0.281927 0.427120 0.016 Uiso 1 1 calc R U . . .
H23B H 0.785530 0.397225 0.472934 0.016 Uiso 1 1 calc R U . . .
C24 C 0.87072(6) 0.4675(2) 0.47172(5) 0.0157(3) Uani 1 1 d . . . . .
C25 C 0.95376(6) 0.3060(3) 0.53110(6) 0.0251(3) Uani 1 1 d . . . . .
H25A H 0.977150 0.344132 0.507744 0.030 Uiso 1 1 calc R U . . .
H25B H 0.966478 0.153974 0.545276 0.030 Uiso 1 1 calc R U . . .
C26 C 0.96598(8) 0.4789(3) 0.57229(7) 0.0332(4) Uani 1 1 d . . . . .
H26A H 0.954789 0.630349 0.558218 0.050 Uiso 1 1 calc R U . . .
H26B H 1.008272 0.477342 0.590029 0.050 Uiso 1 1 calc R U . . .
H26C H 0.942845 0.441554 0.595445 0.050 Uiso 1 1 calc R U . . .
C27 C 0.91284(6) 0.0709(3) 0.30100(5) 0.0177(3) Uani 1 1 d . . . . .
C28 C 0.94705(7) -0.0229(3) 0.35211(6) 0.0235(3) Uani 1 1 d . . . . .
H28A H 0.953591 0.099403 0.376818 0.035 Uiso 1 1 calc R U . . .
H28B H 0.985322 -0.082977 0.350386 0.035 Uiso 1 1 calc R U . . .
H28C H 0.924054 -0.144884 0.361738 0.035 Uiso 1 1 calc R U . . .
C29 C 0.90497(7) -0.1222(3) 0.26287(6) 0.0286(3) Uani 1 1 d . . . . .
H29A H 0.882114 -0.245696 0.272119 0.043 Uiso 1 1 calc R U . . .
H29B H 0.943929 -0.179420 0.262269 0.043 Uiso 1 1 calc R U . . .
H29C H 0.883829 -0.064799 0.229853 0.043 Uiso 1 1 calc R U . . .
C30 C 0.95026(6) 0.2585(3) 0.28622(6) 0.0242(3) Uani 1 1 d . . . . .
H30A H 0.929427 0.317255 0.253259 0.036 Uiso 1 1 calc R U . . .
H30B H 0.988589 0.195476 0.285404 0.036 Uiso 1 1 calc R U . . .
H30C H 0.956623 0.382183 0.310575 0.036 Uiso 1 1 calc R U . . .
C31 C 0.68534(6) 0.0531(2) 0.24988(5) 0.0144(2) Uani 1 1 d . . . . .
C32 C 0.69560(6) -0.1440(2) 0.21723(5) 0.0199(3) Uani 1 1 d . . . . .
H32A H 0.716789 -0.087744 0.193998 0.030 Uiso 1 1 calc R U . . .
H32B H 0.657350 -0.207458 0.198517 0.030 Uiso 1 1 calc R U . . .
H32C H 0.719215 -0.262436 0.238333 0.030 Uiso 1 1 calc R U . . .
C33 C 0.64791(6) 0.2352(2) 0.21550(5) 0.0181(3) Uani 1 1 d . . . . .
H33A H 0.640106 0.361591 0.235608 0.027 Uiso 1 1 calc R U . . .
H33B H 0.610268 0.168247 0.196427 0.027 Uiso 1 1 calc R U . . .
H33C H 0.669558 0.291547 0.192621 0.027 Uiso 1 1 calc R U . . .
C34 C 0.65031(6) -0.0426(2) 0.28433(5) 0.0166(3) Uani 1 1 d . . . . .
H34A H 0.672650 -0.167350 0.304156 0.025 Uiso 1 1 calc R U . . .
H34B H 0.611886 -0.099286 0.264268 0.025 Uiso 1 1 calc R U . . .
H34C H 0.644073 0.077964 0.306509 0.025 Uiso 1 1 calc R U . . .
C35 C 0.58238(6) 0.2285(3) 0.39018(5) 0.0232(3) Uani 1 1 d . . . . .
H35 H 0.606780 0.188151 0.422169 0.028 Uiso 1 1 calc R U . . .
C36 C 0.52698(7) 0.1301(3) 0.37306(6) 0.0293(3) Uani 1 1 d . . . . .
H36 H 0.513805 0.021988 0.392841 0.035 Uiso 1 1 calc R U . . .
C37 C 0.49109(6) 0.1908(3) 0.32694(6) 0.0290(3) Uani 1 1 d . . . . .
H37 H 0.452712 0.126542 0.314626 0.035 Uiso 1 1 calc R U . . .
C38 C 0.51200(6) 0.3468(3) 0.29896(6) 0.0286(3) Uani 1 1 d . . . . .
H38 H 0.488078 0.391975 0.267135 0.034 Uiso 1 1 calc R U . . .
C39 C 0.56815(6) 0.4363(3) 0.31787(5) 0.0214(3) Uani 1 1 d . . . . .
H39 H 0.582733 0.541440 0.298347 0.026 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 2.0002(9) . ?
Pd1 O2 1.9853(9) . ?
Pd1 N1 2.0462(10) . ?
Pd1 N2 2.0386(11) . ?
O1 C1 1.3390(15) . ?
O2 C10 1.3344(16) . ?
O3 C24 1.2036(17) . ?
O4 C24 1.3385(17) . ?
O4 C25 1.4612(16) . ?
N1 C7 1.5096(15) . ?
N1 C8 1.4934(16) . ?
N1 C23 1.4820(16) . ?
N2 C35 1.3382(19) . ?
N2 C39 1.3401(18) . ?
C1 C2 1.4168(18) . ?
C1 C6 1.4083(18) . ?
C2 C3 1.3997(18) . ?
C2 C31 1.5370(17) . ?
C3 H3 0.9500 . ?
C3 C4 1.3978(18) . ?
C4 C5 1.3942(19) . ?
C4 C27 1.5348(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.3897(18) . ?
C6 C7 1.5002(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.5075(17) . ?
C9 C10 1.4122(18) . ?
C9 C18 1.3943(18) . ?
C10 C11 1.4212(18) . ?
C11 C12 1.5398(17) . ?
C11 C16 1.3951(18) . ?
C12 C13 1.538(2) . ?
C12 C14 1.5440(18) . ?
C12 C15 1.5346(18) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C16 C17 1.3965(18) . ?
C17 C18 1.3910(18) . ?
C17 C19 1.5378(18) . ?
C18 H18 0.9500 . ?
C19 C20 1.527(2) . ?
C19 C21 1.537(2) . ?
C19 C22 1.532(2) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.5170(18) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.504(2) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.536(2) . ?
C27 C29 1.534(2) . ?
C27 C30 1.537(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.5362(19) . ?
C31 C33 1.5419(18) . ?
C31 C34 1.5383(18) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35 0.9500 . ?
C35 C36 1.383(2) . ?
C36 H36 0.9500 . ?
C36 C37 1.379(2) . ?
C37 H37 0.9500 . ?
C37 C38 1.383(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.382(2) . ?
C39 H39 0.9500 . ?

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
O1 Pd1 N1 94.45(4) . . ?
O1 Pd1 N2 85.84(4) . . ?
O2 Pd1 O1 172.28(4) . . ?
O2 Pd1 N1 93.12(4) . . ?
O2 Pd1 N2 86.66(4) . . ?
N2 Pd1 N1 177.81(4) . . ?
C1 O1 Pd1 119.92(7) . . ?
C10 O2 Pd1 127.41(8) . . ?
C24 O4 C25 116.54(11) . . ?
C7 N1 Pd1 109.11(7) . . ?
C8 N1 Pd1 107.16(7) . . ?
C8 N1 C7 108.56(9) . . ?
C23 N1 Pd1 106.63(7) . . ?
C23 N1 C7 112.48(10) . . ?
C23 N1 C8 112.70(10) . . ?
C35 N2 Pd1 120.11(9) . . ?
C35 N2 C39 119.08(12) . . ?
C39 N2 Pd1 120.60(10) . . ?
O1 C1 C2 120.97(11) . . ?
O1 C1 C6 119.91(12) . . ?
C6 C1 C2 119.09(11) . . ?
C1 C2 C31 120.62(11) . . ?
C3 C2 C1 117.73(11) . . ?
C3 C2 C31 121.65(12) . . ?
C2 C3 H3 118.1 . . ?
C4 C3 C2 123.80(12) . . ?
C4 C3 H3 118.1 . . ?
C3 C4 C27 122.87(12) . . ?
C5 C4 C3 117.05(12) . . ?
C5 C4 C27 120.07(12) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.34(12) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C7 118.37(11) . . ?
C5 C6 C1 120.88(12) . . ?
C5 C6 C7 120.67(11) . . ?
N1 C7 H7A 109.0 . . ?
N1 C7 H7B 109.0 . . ?
C6 C7 N1 112.88(10) . . ?
C6 C7 H7A 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
N1 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 . . ?
N1 C8 C9 115.23(10) . . ?
H8A C8 H8B 107.5 . . ?
C9 C8 H8A 108.5 . . ?
C9 C8 H8B 108.5 . . ?
C10 C9 C8 122.01(11) . . ?
C18 C9 C8 117.46(11) . . ?
C18 C9 C10 120.39(11) . . ?
O2 C10 C9 122.90(11) . . ?
O2 C10 C11 118.79(11) . . ?
C9 C10 C11 118.31(11) . . ?
C10 C11 C12 120.10(11) . . ?
C16 C11 C10 118.44(11) . . ?
C16 C11 C12 121.46(11) . . ?
C11 C12 C14 110.04(11) . . ?
C13 C12 C11 109.83(10) . . ?
C13 C12 C14 110.77(11) . . ?
C15 C12 C11 112.41(11) . . ?
C15 C12 C13 107.23(11) . . ?
C15 C12 C14 106.48(11) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16 118.1 . . ?
C11 C16 C17 123.79(12) . . ?
C17 C16 H16 118.1 . . ?
C16 C17 C19 123.36(11) . . ?
C18 C17 C16 116.53(12) . . ?
C18 C17 C19 120.07(12) . . ?
C9 C18 H18 118.9 . . ?
C17 C18 C9 122.17(12) . . ?
C17 C18 H18 118.9 . . ?
C20 C19 C17 112.10(12) . . ?
C20 C19 C21 107.14(13) . . ?
C20 C19 C22 109.40(14) . . ?
C21 C19 C17 110.05(12) . . ?
C22 C19 C17 109.28(12) . . ?
C22 C19 C21 108.81(12) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 H23A 108.2 . . ?
N1 C23 H23B 108.2 . . ?
N1 C23 C24 116.51(11) . . ?
H23A C23 H23B 107.3 . . ?
C24 C23 H23A 108.2 . . ?
C24 C23 H23B 108.2 . . ?
O3 C24 O4 124.58(13) . . ?
O3 C24 C23 127.36(13) . . ?
O4 C24 C23 108.04(11) . . ?
O4 C25 H25A 109.3 . . ?
O4 C25 H25B 109.3 . . ?
O4 C25 C26 111.54(13) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C4 C27 C28 109.31(11) . . ?
C4 C27 C30 110.36(12) . . ?
C28 C27 C30 108.55(12) . . ?
C29 C27 C4 112.15(11) . . ?
C29 C27 C28 108.28(13) . . ?
C29 C27 C30 108.11(12) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C2 C31 C33 109.97(11) . . ?
C2 C31 C34 110.25(10) . . ?
C32 C31 C2 111.76(11) . . ?
C32 C31 C33 107.99(11) . . ?
C32 C31 C34 107.30(11) . . ?
C34 C31 C33 109.49(11) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C35 H35 119.1 . . ?
N2 C35 C36 121.88(14) . . ?
C36 C35 H35 119.1 . . ?
C35 C36 H36 120.4 . . ?
C37 C36 C35 119.23(15) . . ?
C37 C36 H36 120.4 . . ?
C36 C37 H37 120.6 . . ?
C36 C37 C38 118.78(14) . . ?
C38 C37 H37 120.6 . . ?
C37 C38 H38 120.4 . . ?
C39 C38 C37 119.16(14) . . ?
C39 C38 H38 120.4 . . ?
N2 C39 C38 121.86(14) . . ?
N2 C39 H39 119.1 . . ?
C38 C39 H39 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C1 C2 137.05(10) . . . . ?
Pd1 O1 C1 C6 -45.17(15) . . . . ?
Pd1 O2 C10 C9 0.5(2) . . . . ?
Pd1 O2 C10 C11 -179.55(9) . . . . ?
Pd1 N1 C7 C6 -61.68(11) . . . . ?
Pd1 N1 C8 C9 66.87(11) . . . . ?
Pd1 N1 C23 C24 -178.55(9) . . . . ?
Pd1 N2 C35 C36 -174.74(12) . . . . ?
Pd1 N2 C39 C38 175.76(12) . . . . ?
O1 C1 C2 C3 -179.54(11) . . . . ?
O1 C1 C2 C31 1.05(18) . . . . ?
O1 C1 C6 C5 178.35(11) . . . . ?
O1 C1 C6 C7 -4.70(18) . . . . ?
O2 C10 C11 C12 -5.91(19) . . . . ?
O2 C10 C11 C16 173.96(12) . . . . ?
N1 C8 C9 C10 -50.91(16) . . . . ?
N1 C8 C9 C18 133.46(12) . . . . ?
N1 C23 C24 O3 -8.2(2) . . . . ?
N1 C23 C24 O4 173.44(11) . . . . ?
N2 C35 C36 C37 -0.9(3) . . . . ?
C1 C2 C3 C4 0.25(19) . . . . ?
C1 C2 C31 C32 -179.25(12) . . . . ?
C1 C2 C31 C33 60.82(15) . . . . ?
C1 C2 C31 C34 -60.01(16) . . . . ?
C1 C6 C7 N1 65.39(15) . . . . ?
C2 C1 C6 C5 -3.83(19) . . . . ?
C2 C1 C6 C7 173.12(11) . . . . ?
C2 C3 C4 C5 -2.01(19) . . . . ?
C2 C3 C4 C27 177.26(12) . . . . ?
C3 C2 C31 C32 1.36(17) . . . . ?
C3 C2 C31 C33 -118.57(13) . . . . ?
C3 C2 C31 C34 120.60(13) . . . . ?
C3 C4 C5 C6 0.84(19) . . . . ?
C3 C4 C27 C28 -116.47(14) . . . . ?
C3 C4 C27 C29 3.62(19) . . . . ?
C3 C4 C27 C30 124.22(14) . . . . ?
C4 C5 C6 C1 2.05(19) . . . . ?
C4 C5 C6 C7 -174.83(12) . . . . ?
C5 C4 C27 C28 62.78(16) . . . . ?
C5 C4 C27 C29 -177.13(13) . . . . ?
C5 C4 C27 C30 -56.53(16) . . . . ?
C5 C6 C7 N1 -117.65(13) . . . . ?
C6 C1 C2 C3 2.66(18) . . . . ?
C6 C1 C2 C31 -176.75(11) . . . . ?
C7 N1 C8 C9 -175.41(10) . . . . ?
C7 N1 C23 C24 61.89(14) . . . . ?
C8 N1 C7 C6 -178.15(10) . . . . ?
C8 N1 C23 C24 -61.24(14) . . . . ?
C8 C9 C10 O2 11.1(2) . . . . ?
C8 C9 C10 C11 -168.76(12) . . . . ?
C8 C9 C18 C17 173.23(12) . . . . ?
C9 C10 C11 C12 174.00(12) . . . . ?
C9 C10 C11 C16 -6.13(19) . . . . ?
C10 C9 C18 C17 -2.5(2) . . . . ?
C10 C11 C12 C13 67.56(15) . . . . ?
C10 C11 C12 C14 -54.65(16) . . . . ?
C10 C11 C12 C15 -173.14(12) . . . . ?
C10 C11 C16 C17 1.3(2) . . . . ?
C11 C16 C17 C18 2.9(2) . . . . ?
C11 C16 C17 C19 -179.57(13) . . . . ?
C12 C11 C16 C17 -178.79(12) . . . . ?
C16 C11 C12 C13 -112.30(13) . . . . ?
C16 C11 C12 C14 125.49(13) . . . . ?
C16 C11 C12 C15 7.00(18) . . . . ?
C16 C17 C18 C9 -2.3(2) . . . . ?
C16 C17 C19 C20 12.7(2) . . . . ?
C16 C17 C19 C21 131.84(14) . . . . ?
C16 C17 C19 C22 -108.73(15) . . . . ?
C18 C9 C10 O2 -173.34(13) . . . . ?
C18 C9 C10 C11 6.75(19) . . . . ?
C18 C17 C19 C20 -169.85(14) . . . . ?
C18 C17 C19 C21 -50.73(17) . . . . ?
C18 C17 C19 C22 68.70(17) . . . . ?
C19 C17 C18 C9 -179.95(12) . . . . ?
C23 N1 C7 C6 56.43(13) . . . . ?
C23 N1 C8 C9 -50.12(14) . . . . ?
C24 O4 C25 C26 76.80(16) . . . . ?
C25 O4 C24 O3 -0.2(2) . . . . ?
C25 O4 C24 C23 178.18(12) . . . . ?
C27 C4 C5 C6 -178.45(12) . . . . ?
C31 C2 C3 C4 179.65(12) . . . . ?
C35 N2 C39 C38 0.9(2) . . . . ?
C35 C36 C37 C38 0.7(3) . . . . ?
C36 C37 C38 C39 0.3(3) . . . . ?
C37 C38 C39 N2 -1.1(2) . . . . ?
C39 N2 C35 C36 0.1(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_131bg14_0m
_database_code_depnum_ccdc_archive 'CCDC 2063654'
loop_
_audit_author_name
_audit_author_address
'Georgina Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-11-03 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2021-07-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;



# start Validation Reply Form
_vrf_THETM01_131bg14_0m          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Data were reintegrated but the original data was not collected
 to high enough resolution 
It was collected when the  instrument was new, which
 can account for teething issues achieving incomplete datasets.  

;
# end Validation Reply Form
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H62 N2 O4 Pd, C3 H7.5'
_chemical_formula_sum            'C41 H69.50 N2 O4 Pd'
_chemical_formula_weight         760.88
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.3384(7)
_cell_length_b                   9.7533(2)
_cell_length_c                   31.2674(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.1430(10)
_cell_angle_gamma                90
_cell_volume                     8289.3(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      59.871
_cell_measurement_theta_min      4.085
_shelx_estimated_absorpt_T_max   0.859
_shelx_estimated_absorpt_T_min   0.480
_exptl_absorpt_coefficient_mu    3.908
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0712 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.8818.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44289
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        59.916
_diffrn_reflns_theta_max         59.916
_diffrn_reflns_theta_min         2.843
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5449
_reflns_number_total             6054
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 data measured to 0.89 resolution though 2theta range could have been
 extended however existing data gives a good structural model with no
 significant  truncation effects
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6054
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0271
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0255P)²+22.1808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0664
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4S-C2S
 2.5 with sigma of 0.04
3. Others
 Fixed Sof: C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5)
 Fixed Uiso: H4SA(0.08) H4SB(0.08)
4.a Ternary CH refined with riding coordinates:
 N2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C20(H20A,H20B), C35(H35A,H35B),
 C37(H37A,H37B), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C24(H24), C26(H26)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C1S(H1SA,H1SB,H1SC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.28604(2) 0.26119(2) 0.66520(2) 0.01263(7) Uani 1 1 d . . . . .
O1 O 0.22153(6) 0.32161(17) 0.68462(5) 0.0162(4) Uani 1 1 d . . . . .
N1 N 0.28715(7) 0.4149(2) 0.62011(6) 0.0137(4) Uani 1 1 d . . . . .
C1 C 0.25889(9) 0.3761(3) 0.57877(8) 0.0160(5) Uani 1 1 d . . . . .
H1A H 0.225320 0.349004 0.584539 0.019 Uiso 1 1 calc R U . . .
H1B H 0.274653 0.294706 0.567225 0.019 Uiso 1 1 calc R U . . .
O2 O 0.35056(6) 0.17976(18) 0.65374(5) 0.0195(4) Uani 1 1 d . . . . .
N2 N 0.29192(7) 0.1194(2) 0.71414(6) 0.0162(5) Uani 1 1 d . . . . .
H2 H 0.319493 0.056980 0.708390 0.019 Uiso 1 1 calc R U . . .
C2 C 0.25460(9) 0.4870(3) 0.54437(8) 0.0190(6) Uani 1 1 d . . . . .
O3 O 0.27229(7) 0.59987(19) 0.54733(6) 0.0265(4) Uani 1 1 d . . . . .
C3 C 0.21712(11) 0.5340(3) 0.47402(9) 0.0345(8) Uani 1 1 d . . . . .
H3A H 0.211364 0.626851 0.485290 0.041 Uiso 1 1 calc R U . . .
H3B H 0.186944 0.505165 0.455929 0.041 Uiso 1 1 calc R U . . .
O4 O 0.22696(7) 0.4387(2) 0.50991(6) 0.0298(5) Uani 1 1 d . . . . .
C4 C 0.25949(12) 0.5390(3) 0.44694(9) 0.0342(7) Uani 1 1 d . . . . .
H4A H 0.251329 0.600789 0.422506 0.051 Uiso 1 1 calc R U . . .
H4B H 0.265730 0.446791 0.436317 0.051 Uiso 1 1 calc R U . . .
H4C H 0.288956 0.572624 0.464399 0.051 Uiso 1 1 calc R U . . .
C5 C 0.26571(9) 0.5376(2) 0.64044(8) 0.0156(5) Uani 1 1 d . . . . .
H5A H 0.281753 0.548405 0.670165 0.019 Uiso 1 1 calc R U . . .
H5B H 0.272724 0.620861 0.624062 0.019 Uiso 1 1 calc R U . . .
C6 C 0.21124(9) 0.5248(2) 0.64157(7) 0.0146(5) Uani 1 1 d . . . . .
C7 C 0.19196(9) 0.4167(2) 0.66470(7) 0.0144(5) Uani 1 1 d . . . . .
C8 C 0.14040(9) 0.4151(2) 0.66790(8) 0.0150(5) Uani 1 1 d . . . . .
C9 C 0.11137(9) 0.5146(3) 0.64538(8) 0.0180(6) Uani 1 1 d . . . . .
H9 H 0.076923 0.512383 0.647235 0.022 Uiso 1 1 calc R U . . .
C10 C 0.12958(9) 0.6172(3) 0.62036(8) 0.0166(6) Uani 1 1 d . . . . .
C11 C 0.18029(9) 0.6207(2) 0.61964(8) 0.0163(5) Uani 1 1 d . . . . .
H11 H 0.194267 0.690806 0.603698 0.020 Uiso 1 1 calc R U . . .
C12 C 0.11713(9) 0.3057(3) 0.69506(8) 0.0176(6) Uani 1 1 d . . . . .
C13 C 0.12303(10) 0.1641(3) 0.67485(8) 0.0207(6) Uani 1 1 d . . . . .
H13A H 0.103089 0.159676 0.646908 0.031 Uiso 1 1 calc R U . . .
H13B H 0.112089 0.093116 0.693874 0.031 Uiso 1 1 calc R U . . .
H13C H 0.157695 0.148975 0.670861 0.031 Uiso 1 1 calc R U . . .
C14 C 0.14147(9) 0.3085(3) 0.74180(8) 0.0212(6) Uani 1 1 d . . . . .
H14A H 0.177061 0.295960 0.742058 0.032 Uiso 1 1 calc R U . . .
H14B H 0.127937 0.234504 0.758160 0.032 Uiso 1 1 calc R U . . .
H14C H 0.134889 0.396963 0.754933 0.032 Uiso 1 1 calc R U . . .
C15 C 0.06178(9) 0.3298(3) 0.69699(9) 0.0249(6) Uani 1 1 d . . . . .
H15A H 0.056634 0.421826 0.708267 0.037 Uiso 1 1 calc R U . . .
H15B H 0.049063 0.261317 0.715895 0.037 Uiso 1 1 calc R U . . .
H15C H 0.044378 0.321583 0.668027 0.037 Uiso 1 1 calc R U . . .
C16 C 0.09685(9) 0.7228(3) 0.59451(8) 0.0203(6) Uani 1 1 d . . . . .
C17 C 0.10752(10) 0.7204(3) 0.54715(9) 0.0273(6) Uani 1 1 d . . . . .
H17A H 0.141884 0.746139 0.545328 0.041 Uiso 1 1 calc R U . . .
H17B H 0.085797 0.785560 0.530535 0.041 Uiso 1 1 calc R U . . .
H17C H 0.101664 0.627931 0.535442 0.041 Uiso 1 1 calc R U . . .
C18 C 0.10812(11) 0.8667(3) 0.61276(9) 0.0303(7) Uani 1 1 d . . . . .
H18A H 0.101333 0.869595 0.642895 0.045 Uiso 1 1 calc R U . . .
H18B H 0.087383 0.933982 0.596102 0.045 Uiso 1 1 calc R U . . .
H18C H 0.142836 0.888372 0.610951 0.045 Uiso 1 1 calc R U . . .
C19 C 0.04208(10) 0.6938(3) 0.59616(9) 0.0281(7) Uani 1 1 d . . . . .
H19A H 0.034141 0.602510 0.584287 0.042 Uiso 1 1 calc R U . . .
H19B H 0.022532 0.762853 0.579180 0.042 Uiso 1 1 calc R U . . .
H19C H 0.034493 0.697421 0.626069 0.042 Uiso 1 1 calc R U . . .
C20 C 0.34043(8) 0.4409(3) 0.61506(8) 0.0165(5) Uani 1 1 d . . . . .
H20A H 0.343081 0.524078 0.597325 0.020 Uiso 1 1 calc R U . . .
H20B H 0.358407 0.458415 0.643723 0.020 Uiso 1 1 calc R U . . .
C21 C 0.36413(9) 0.3229(3) 0.59441(8) 0.0164(6) Uani 1 1 d . . . . .
C22 C 0.36948(9) 0.1967(3) 0.61628(8) 0.0168(6) Uani 1 1 d . . . . .
C23 C 0.39657(9) 0.0907(3) 0.59866(8) 0.0171(6) Uani 1 1 d . . . . .
C24 C 0.41363(9) 0.1144(3) 0.55868(8) 0.0176(6) Uani 1 1 d . . . . .
H24 H 0.431564 0.043246 0.546645 0.021 Uiso 1 1 calc R U . . .
C25 C 0.40596(9) 0.2359(3) 0.53539(8) 0.0164(6) Uani 1 1 d . . . . .
C26 C 0.38130(8) 0.3397(3) 0.55464(8) 0.0163(6) Uani 1 1 d . . . . .
H26 H 0.376050 0.424755 0.540080 0.020 Uiso 1 1 calc R U . . .
C27 C 0.40787(9) -0.0443(3) 0.62336(8) 0.0211(6) Uani 1 1 d . . . . .
C28 C 0.44025(11) -0.1412(3) 0.59988(9) 0.0314(7) Uani 1 1 d . . . . .
H28A H 0.471345 -0.095375 0.595886 0.047 Uiso 1 1 calc R U . . .
H28B H 0.423122 -0.165407 0.571753 0.047 Uiso 1 1 calc R U . . .
H28C H 0.446960 -0.224533 0.616995 0.047 Uiso 1 1 calc R U . . .
C29 C 0.43602(10) -0.0132(3) 0.66767(8) 0.0260(6) Uani 1 1 d . . . . .
H29A H 0.416199 0.047629 0.683870 0.039 Uiso 1 1 calc R U . . .
H29B H 0.467304 0.031680 0.663730 0.039 Uiso 1 1 calc R U . . .
H29C H 0.442460 -0.098965 0.683595 0.039 Uiso 1 1 calc R U . . .
C30 C 0.35986(10) -0.1217(3) 0.62918(9) 0.0258(6) Uani 1 1 d . . . . .
H30A H 0.367124 -0.199231 0.648765 0.039 Uiso 1 1 calc R U . . .
H30B H 0.345137 -0.155584 0.601223 0.039 Uiso 1 1 calc R U . . .
H30C H 0.336797 -0.059388 0.641267 0.039 Uiso 1 1 calc R U . . .
C31 C 0.42194(9) 0.2553(3) 0.49016(8) 0.0203(6) Uani 1 1 d . . . . .
C32 C 0.44629(14) 0.3946(3) 0.48677(11) 0.0475(9) Uani 1 1 d . . . . .
H32A H 0.421902 0.467124 0.489040 0.071 Uiso 1 1 calc R U . . .
H32B H 0.459648 0.401787 0.458994 0.071 Uiso 1 1 calc R U . . .
H32C H 0.473007 0.404514 0.510084 0.071 Uiso 1 1 calc R U . . .
C33 C 0.46013(11) 0.1490(3) 0.47987(9) 0.0324(7) Uani 1 1 d . . . . .
H33A H 0.469119 0.164775 0.450764 0.049 Uiso 1 1 calc R U . . .
H33B H 0.446251 0.056765 0.481629 0.049 Uiso 1 1 calc R U . . .
H33C H 0.489480 0.157302 0.500636 0.049 Uiso 1 1 calc R U . . .
C34 C 0.37702(12) 0.2415(5) 0.45735(10) 0.0538(11) Uani 1 1 d . . . . .
H34A H 0.353123 0.313055 0.462348 0.081 Uiso 1 1 calc R U . . .
H34B H 0.362031 0.151138 0.460237 0.081 Uiso 1 1 calc R U . . .
H34C H 0.386939 0.251322 0.428301 0.081 Uiso 1 1 calc R U . . .
C35 C 0.24849(9) 0.0298(3) 0.71703(8) 0.0190(6) Uani 1 1 d . . . . .
H35A H 0.219672 0.086968 0.721872 0.023 Uiso 1 1 calc R U . . .
H35B H 0.255069 -0.033029 0.741843 0.023 Uiso 1 1 calc R U . . .
C36 C 0.23700(10) -0.0529(3) 0.67646(8) 0.0230(6) Uani 1 1 d . . . . .
H36A H 0.233657 0.008791 0.651568 0.035 Uiso 1 1 calc R U . . .
H36B H 0.206152 -0.103051 0.677818 0.035 Uiso 1 1 calc R U . . .
H36C H 0.263732 -0.118085 0.673611 0.035 Uiso 1 1 calc R U . . .
C37 C 0.30740(9) 0.1859(3) 0.75626(8) 0.0205(6) Uani 1 1 d . . . . .
H37A H 0.312403 0.114465 0.778795 0.025 Uiso 1 1 calc R U . . .
H37B H 0.280789 0.247369 0.763775 0.025 Uiso 1 1 calc R U . . .
C38 C 0.35411(10) 0.2676(3) 0.75573(9) 0.0294(7) Uani 1 1 d . . . . .
H38A H 0.348310 0.344710 0.735722 0.044 Uiso 1 1 calc R U . . .
H38B H 0.380022 0.208723 0.746452 0.044 Uiso 1 1 calc R U . . .
H38C H 0.364370 0.302656 0.784686 0.044 Uiso 1 1 calc R U . . .
C1S C 0.47487(14) 0.4941(4) 0.66111(14) 0.0626(11) Uani 1 1 d . . . . .
H1SA H 0.462585 0.579491 0.672589 0.094 Uiso 1 1 calc R U . A .
H1SB H 0.455979 0.472904 0.633484 0.094 Uiso 1 1 calc R U . . .
H1SC H 0.509688 0.504941 0.656942 0.094 Uiso 1 1 calc R U . . .
C2S C 0.46946(19) 0.3823(5) 0.69145(18) 0.0898(16) Uani 1 1 d D . . A -1
H2SA H 0.438810 0.405050 0.704149 0.108 Uiso 1 1 calc R U . A -1
H2SB H 0.461243 0.301753 0.672777 0.108 Uiso 1 1 calc R U . A -1
C3S C 0.4978(3) 0.3335(8) 0.7231(3) 0.0521(19) Uani 0.5 1 d . . P A -1
H3SA H 0.531748 0.324662 0.715190 0.063 Uiso 0.5 1 calc R U P A -1
H3SB H 0.486184 0.241707 0.730993 0.063 Uiso 0.5 1 calc R U P A -1
H4SA H 0.4630(16) 0.450(4) 0.7666(13) 0.080 Uiso 1 1 d . U . . .
C4S C 0.4966(4) 0.4356(9) 0.7620(3) 0.052(3) Uani 0.5 1 d D . P A -1
H4SB H 0.500000 0.545(7) 0.750000 0.080 Uiso 1 2 d S U P . .


_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 O1 2.0138(16) . ?
Pd1 N1 2.061(2) . ?
Pd1 O2 2.0013(16) . ?
Pd1 N2 2.056(2) . ?
O1 C7 1.339(3) . ?
N1 C1 1.482(3) . ?
N1 C5 1.503(3) . ?
N1 C20 1.503(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.520(3) . ?
O2 C22 1.340(3) . ?
N2 H2 1.0000 . ?
N2 C35 1.485(3) . ?
N2 C37 1.489(3) . ?
C2 O3 1.202(3) . ?
C2 O4 1.334(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 O4 1.460(3) . ?
C3 C4 1.507(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.498(3) . ?
C6 C7 1.412(3) . ?
C6 C11 1.392(3) . ?
C7 C8 1.424(3) . ?
C8 C9 1.396(3) . ?
C8 C12 1.542(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(4) . ?
C10 C11 1.389(3) . ?
C10 C16 1.537(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.535(4) . ?
C12 C14 1.540(4) . ?
C12 C15 1.539(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.540(4) . ?
C16 C18 1.533(4) . ?
C16 C19 1.530(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.500(3) . ?
C21 C22 1.409(4) . ?
C21 C26 1.385(3) . ?
C22 C23 1.417(4) . ?
C23 C24 1.399(3) . ?
C23 C27 1.541(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.395(4) . ?
C25 C26 1.389(4) . ?
C25 C31 1.536(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.534(4) . ?
C27 C29 1.542(4) . ?
C27 C30 1.541(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.521(4) . ?
C31 C33 1.530(4) . ?
C31 C34 1.520(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.507(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.507(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C1S C2S 1.464(6) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C2S C3S 1.281(8) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.574(10) . ?
C4S H4SA 0.95(4) . ?
C4S H4SB 1.14(6) . ?

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
O1 Pd1 N1 94.06(7) . . ?
O1 Pd1 N2 88.49(7) . . ?
O2 Pd1 O1 170.79(6) . . ?
O2 Pd1 N1 95.08(7) . . ?
O2 Pd1 N2 82.30(7) . . ?
N2 Pd1 N1 173.20(8) . . ?
C7 O1 Pd1 124.54(14) . . ?
C1 N1 Pd1 111.50(14) . . ?
C1 N1 C5 112.43(18) . . ?
C1 N1 C20 111.82(18) . . ?
C5 N1 Pd1 104.77(14) . . ?
C5 N1 C20 109.68(18) . . ?
C20 N1 Pd1 106.24(14) . . ?
N1 C1 H1A 108.4 . . ?
N1 C1 H1B 108.4 . . ?
N1 C1 C2 115.4(2) . . ?
H1A C1 H1B 107.5 . . ?
C2 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
C22 O2 Pd1 122.52(15) . . ?
Pd1 N2 H2 106.0 . . ?
C35 N2 Pd1 116.22(15) . . ?
C35 N2 H2 106.0 . . ?
C35 N2 C37 110.87(19) . . ?
C37 N2 Pd1 110.94(15) . . ?
C37 N2 H2 106.0 . . ?
O3 C2 C1 126.6(2) . . ?
O3 C2 O4 125.0(2) . . ?
O4 C2 C1 108.3(2) . . ?
H3A C3 H3B 108.0 . . ?
O4 C3 H3A 109.4 . . ?
O4 C3 H3B 109.4 . . ?
O4 C3 C4 111.3(2) . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C2 O4 C3 116.0(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5A 109.2 . . ?
N1 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 N1 112.17(19) . . ?
C6 C5 H5A 109.2 . . ?
C6 C5 H5B 109.2 . . ?
C7 C6 C5 120.0(2) . . ?
C11 C6 C5 119.1(2) . . ?
C11 C6 C7 120.9(2) . . ?
O1 C7 C6 121.0(2) . . ?
O1 C7 C8 120.8(2) . . ?
C6 C7 C8 118.1(2) . . ?
C7 C8 C12 121.1(2) . . ?
C9 C8 C7 118.1(2) . . ?
C9 C8 C12 120.9(2) . . ?
C8 C9 H9 117.8 . . ?
C10 C9 C8 124.4(2) . . ?
C10 C9 H9 117.8 . . ?
C9 C10 C16 123.6(2) . . ?
C11 C10 C9 116.3(2) . . ?
C11 C10 C16 120.0(2) . . ?
C6 C11 H11 119.0 . . ?
C10 C11 C6 122.0(2) . . ?
C10 C11 H11 119.0 . . ?
C13 C12 C8 109.1(2) . . ?
C13 C12 C14 110.7(2) . . ?
C13 C12 C15 107.5(2) . . ?
C14 C12 C8 110.4(2) . . ?
C15 C12 C8 112.4(2) . . ?
C15 C12 C14 106.7(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C16 C17 109.6(2) . . ?
C18 C16 C10 109.6(2) . . ?
C18 C16 C17 108.7(2) . . ?
C19 C16 C10 112.0(2) . . ?
C19 C16 C17 108.4(2) . . ?
C19 C16 C18 108.4(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.1 . . ?
N1 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 N1 112.6(2) . . ?
C21 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C22 C21 C20 119.3(2) . . ?
C26 C21 C20 120.0(2) . . ?
C26 C21 C22 120.7(2) . . ?
O2 C22 C21 120.1(2) . . ?
O2 C22 C23 121.1(2) . . ?
C21 C22 C23 118.7(2) . . ?
C22 C23 C27 120.9(2) . . ?
C24 C23 C22 117.7(2) . . ?
C24 C23 C27 121.4(2) . . ?
C23 C24 H24 117.9 . . ?
C25 C24 C23 124.1(2) . . ?
C25 C24 H24 117.9 . . ?
C24 C25 C31 123.0(2) . . ?
C26 C25 C24 116.5(2) . . ?
C26 C25 C31 120.5(2) . . ?
C21 C26 C25 122.0(2) . . ?
C21 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C23 C27 C29 109.6(2) . . ?
C23 C27 C30 110.5(2) . . ?
C28 C27 C23 112.4(2) . . ?
C28 C27 C29 107.1(2) . . ?
C28 C27 C30 107.3(2) . . ?
C30 C27 C29 109.9(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C25 110.1(2) . . ?
C32 C31 C33 106.1(2) . . ?
C33 C31 C25 112.2(2) . . ?
C34 C31 C25 108.8(2) . . ?
C34 C31 C32 111.1(3) . . ?
C34 C31 C33 108.5(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C35 H35A 109.4 . . ?
N2 C35 H35B 109.4 . . ?
N2 C35 C36 111.1(2) . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 H37A 109.1 . . ?
N2 C37 H37B 109.1 . . ?
N2 C37 C38 112.5(2) . . ?
H37A C37 H37B 107.8 . . ?
C38 C37 H37A 109.1 . . ?
C38 C37 H37B 109.1 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
C1S C2S H2SA 104.0 . . ?
C1S C2S H2SB 104.0 . . ?
H2SA C2S H2SB 105.4 . . ?
C3S C2S C1S 133.1(6) . . ?
C3S C2S H2SA 104.0 . . ?
C3S C2S H2SB 104.0 . . ?
C2S C3S H3SA 110.2 . . ?
C2S C3S H3SB 110.2 . . ?
C2S C3S C4S 107.5(7) . . ?
H3SA C3S H3SB 108.5 . . ?
C4S C3S H3SA 110.2 . . ?
C4S C3S H3SB 110.2 . . ?
C3S C4S H4SA 108(3) . . ?
C3S C4S H4SB 109.3(14) . . ?
H4SA C4S H4SB 91(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C7 C6 -29.4(3) . . . . ?
Pd1 O1 C7 C8 153.47(17) . . . . ?
Pd1 N1 C1 C2 175.97(16) . . . . ?
Pd1 N1 C5 C6 -73.1(2) . . . . ?
Pd1 N1 C20 C21 68.0(2) . . . . ?
Pd1 O2 C22 C21 37.6(3) . . . . ?
Pd1 O2 C22 C23 -144.62(19) . . . . ?
Pd1 N2 C35 C36 60.0(2) . . . . ?
Pd1 N2 C37 C38 -54.5(2) . . . . ?
O1 C7 C8 C9 -178.2(2) . . . . ?
O1 C7 C8 C12 1.2(3) . . . . ?
N1 C1 C2 O3 1.3(4) . . . . ?
N1 C1 C2 O4 -177.9(2) . . . . ?
N1 C5 C6 C7 61.5(3) . . . . ?
N1 C5 C6 C11 -118.6(2) . . . . ?
N1 C20 C21 C22 -65.4(3) . . . . ?
N1 C20 C21 C26 115.7(2) . . . . ?
C1 N1 C5 C6 48.1(3) . . . . ?
C1 N1 C20 C21 -53.9(3) . . . . ?
C1 C2 O4 C3 177.6(2) . . . . ?
O2 C22 C23 C24 177.7(2) . . . . ?
O2 C22 C23 C27 -3.8(4) . . . . ?
O3 C2 O4 C3 -1.6(4) . . . . ?
C4 C3 O4 C2 81.8(3) . . . . ?
C5 N1 C1 C2 58.7(3) . . . . ?
C5 N1 C20 C21 -179.32(19) . . . . ?
C5 C6 C7 O1 -2.4(3) . . . . ?
C5 C6 C7 C8 174.8(2) . . . . ?
C5 C6 C11 C10 -178.2(2) . . . . ?
C6 C7 C8 C9 4.6(3) . . . . ?
C6 C7 C8 C12 -176.0(2) . . . . ?
C7 C6 C11 C10 1.8(4) . . . . ?
C7 C8 C9 C10 -1.0(4) . . . . ?
C7 C8 C12 C13 -65.4(3) . . . . ?
C7 C8 C12 C14 56.4(3) . . . . ?
C7 C8 C12 C15 175.4(2) . . . . ?
C8 C9 C10 C11 -2.3(4) . . . . ?
C8 C9 C10 C16 177.8(2) . . . . ?
C9 C8 C12 C13 114.0(2) . . . . ?
C9 C8 C12 C14 -124.2(2) . . . . ?
C9 C8 C12 C15 -5.2(3) . . . . ?
C9 C10 C11 C6 1.9(3) . . . . ?
C9 C10 C16 C17 -125.8(3) . . . . ?
C9 C10 C16 C18 115.0(3) . . . . ?
C9 C10 C16 C19 -5.3(3) . . . . ?
C11 C6 C7 O1 177.7(2) . . . . ?
C11 C6 C7 C8 -5.1(3) . . . . ?
C11 C10 C16 C17 54.3(3) . . . . ?
C11 C10 C16 C18 -64.9(3) . . . . ?
C11 C10 C16 C19 174.8(2) . . . . ?
C12 C8 C9 C10 179.7(2) . . . . ?
C16 C10 C11 C6 -178.2(2) . . . . ?
C20 N1 C1 C2 -65.2(3) . . . . ?
C20 N1 C5 C6 173.22(19) . . . . ?
C20 C21 C22 O2 4.5(3) . . . . ?
C20 C21 C22 C23 -173.3(2) . . . . ?
C20 C21 C26 C25 176.3(2) . . . . ?
C21 C22 C23 C24 -4.5(3) . . . . ?
C21 C22 C23 C27 174.0(2) . . . . ?
C22 C21 C26 C25 -2.5(4) . . . . ?
C22 C23 C24 C25 0.5(4) . . . . ?
C22 C23 C27 C28 -176.4(2) . . . . ?
C22 C23 C27 C29 -57.5(3) . . . . ?
C22 C23 C27 C30 63.7(3) . . . . ?
C23 C24 C25 C26 2.4(4) . . . . ?
C23 C24 C25 C31 -175.6(2) . . . . ?
C24 C23 C27 C28 2.0(3) . . . . ?
C24 C23 C27 C29 120.9(3) . . . . ?
C24 C23 C27 C30 -117.8(3) . . . . ?
C24 C25 C26 C21 -1.5(4) . . . . ?
C24 C25 C31 C32 -135.8(3) . . . . ?
C24 C25 C31 C33 -17.9(3) . . . . ?
C24 C25 C31 C34 102.2(3) . . . . ?
C26 C21 C22 O2 -176.7(2) . . . . ?
C26 C21 C22 C23 5.5(4) . . . . ?
C26 C25 C31 C32 46.2(3) . . . . ?
C26 C25 C31 C33 164.2(2) . . . . ?
C26 C25 C31 C34 -75.8(3) . . . . ?
C27 C23 C24 C25 -177.9(2) . . . . ?
C31 C25 C26 C21 176.6(2) . . . . ?
C35 N2 C37 C38 174.8(2) . . . . ?
C37 N2 C35 C36 -172.1(2) . . . . ?
C1S C2S C3S C4S 76.4(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_cu_8v00517_0m
_database_code_depnum_ccdc_archive 'CCDC 2070849'
loop_
_audit_author_name
_audit_author_address
'Georgina Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-11-10 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT097_cu_8v00517_0m       
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       1.34 eA-3
RESPONSE: Residual peaks are found which are approximately 1 \%A in height, 1.25 \%A apart, angle at central atom 90\%. From the geometry this is most likely disordered methanol, which is close to a disordered ethyl substituent. Since the peaks are very close to the main molecule, our attempts on masking did not work. The solvent molecule was assumed to be 0.5 MeOH which adds 0.5 C 0.5 O and 2 H to the asymmetric unit, and 2 C 2 O and 8 H to the unit cell. It was modelled as carbon atoms with 1/3 occupancy. Modelling one position as oxygen did not improve the model.
;
# Added during the CSD deposition process: Wednesday 10 November 2021 04:18 PM
# end Validation Reply Form

_audit_creation_date             2021-03-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C41 H59 N O4'
_chemical_formula_sum            'C41 H59 N O4'
_chemical_formula_weight         629.89
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.4115(2)
_cell_length_b                   11.7529(2)
_cell_length_c                   31.8349(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3895.49(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.376
_cell_measurement_theta_min      3.761
_shelx_estimated_absorpt_T_max   0.930
_shelx_estimated_absorpt_T_min   0.880
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0985 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.8951. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            48693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.371
_diffrn_reflns_theta_min         4.009
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6960
_reflns_number_total             7128
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_refine_diff_density_max         1.342
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
 Flack x determined using 2936 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0567
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0960P)²+2.4815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1632
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C34A-C33 \\sim C34-C33
 with sigma of 0.02
3. Others
 Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C31(H31)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B), C33(H33A,H33B), C33(H33C,H33D), C35(H35A,H35B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C20(H20), C22(H22), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F)
4.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1867(2) 0.8589(2) 0.42817(8) 0.0276(5) Uani 1 1 d . . . . .
H1 H 0.229190 0.801880 0.435874 0.041 Uiso 1 1 calc GR . . . .
N1 N 0.4453(3) 0.7259(2) 0.40771(8) 0.0207(6) Uani 1 1 d . . . . .
C1 C 0.4594(3) 0.8222(3) 0.43731(10) 0.0226(7) Uani 1 1 d . . . . .
H1A H 0.551612 0.834736 0.443254 0.027 Uiso 1 1 calc R . . . .
H1B H 0.416243 0.803190 0.464126 0.027 Uiso 1 1 calc R . . . .
O2 O 0.2652(2) 0.6700(2) 0.34961(7) 0.0277(5) Uani 1 1 d . . . . .
H2 H 0.295577 0.702849 0.370830 0.042 Uiso 1 1 calc GR . . . .
C2 C 0.4018(3) 0.9300(3) 0.41962(10) 0.0229(7) Uani 1 1 d . . . . .
O3 O 0.2488(2) 0.6407(2) 0.45545(8) 0.0293(6) Uani 1 1 d . . . . .
C3 C 0.2690(3) 0.9429(3) 0.41529(10) 0.0223(7) Uani 1 1 d . . . . .
O4 O 0.3427(3) 0.4695(2) 0.46002(10) 0.0382(7) Uani 1 1 d . . . . .
C4 C 0.2162(3) 1.0429(3) 0.39765(10) 0.0241(7) Uani 1 1 d . . . . .
C5 C 0.3033(3) 1.1277(3) 0.38525(10) 0.0247(7) Uani 1 1 d . . . . .
H5 H 0.269534 1.195644 0.373402 0.030 Uiso 1 1 calc R . . . .
C6 C 0.4365(3) 1.1183(3) 0.38930(10) 0.0248(7) Uani 1 1 d . . . . .
C7 C 0.4827(3) 1.0175(3) 0.40668(11) 0.0240(7) Uani 1 1 d . . . . .
H7 H 0.572873 1.008129 0.409811 0.029 Uiso 1 1 calc R . . . .
C8 C 0.0705(4) 1.0582(3) 0.39231(11) 0.0276(7) Uani 1 1 d . . . . .
C9 C 0.0159(4) 0.9647(4) 0.36364(12) 0.0330(8) Uani 1 1 d . . . . .
H9A H 0.053667 0.971637 0.335560 0.049 Uiso 1 1 calc GR . . . .
H9B H -0.077601 0.973043 0.361709 0.049 Uiso 1 1 calc GR . . . .
H9C H 0.036692 0.889849 0.375366 0.049 Uiso 1 1 calc GR . . . .
C10 C 0.0361(4) 1.1739(4) 0.37263(13) 0.0357(9) Uani 1 1 d . . . . .
H10A H 0.069016 1.235273 0.390477 0.054 Uiso 1 1 calc GR . . . .
H10B H -0.057390 1.180535 0.370237 0.054 Uiso 1 1 calc GR . . . .
H10C H 0.074930 1.179489 0.344660 0.054 Uiso 1 1 calc GR . . . .
C11 C 0.0038(4) 1.0535(4) 0.43577(12) 0.0334(8) Uani 1 1 d . . . . .
H11A H 0.025840 0.981978 0.449827 0.050 Uiso 1 1 calc GR . . . .
H11B H -0.089448 1.058004 0.432005 0.050 Uiso 1 1 calc GR . . . .
H11C H 0.032921 1.117733 0.452962 0.050 Uiso 1 1 calc GR . . . .
C12 C 0.5311(4) 1.2101(3) 0.37577(13) 0.0334(8) Uani 1 1 d . . . . .
C13 C 0.4661(4) 1.3159(3) 0.35892(14) 0.0382(9) Uani 1 1 d . . . . .
H13A H 0.415526 1.296305 0.333989 0.057 Uiso 1 1 calc GR . . . .
H13B H 0.531354 1.372427 0.351375 0.057 Uiso 1 1 calc GR . . . .
H13C H 0.409267 1.347602 0.380510 0.057 Uiso 1 1 calc GR . . . .
C14 C 0.6127(6) 1.2461(4) 0.41460(18) 0.0597(15) Uani 1 1 d . . . . .
H14A H 0.556645 1.280844 0.435755 0.090 Uiso 1 1 calc GR . . . .
H14B H 0.678069 1.301285 0.405869 0.090 Uiso 1 1 calc GR . . . .
H14C H 0.654703 1.178966 0.426591 0.090 Uiso 1 1 calc GR . . . .
C15 C 0.6218(5) 1.1613(4) 0.34264(18) 0.0512(12) Uani 1 1 d . . . . .
H15A H 0.665786 1.094417 0.354113 0.077 Uiso 1 1 calc GR . . . .
H15B H 0.685361 1.218938 0.334807 0.077 Uiso 1 1 calc GR . . . .
H15C H 0.572323 1.139047 0.317764 0.077 Uiso 1 1 calc GR . . . .
C16 C 0.5212(3) 0.7442(3) 0.36895(10) 0.0217(7) Uani 1 1 d . . . . .
H16A H 0.613764 0.739266 0.375900 0.026 Uiso 1 1 calc R . . . .
H16B H 0.504192 0.821788 0.358237 0.026 Uiso 1 1 calc R . . . .
C17 C 0.4909(3) 0.6588(3) 0.33468(10) 0.0215(7) Uani 1 1 d . . . . .
C18 C 0.3637(3) 0.6282(3) 0.32546(10) 0.0224(7) Uani 1 1 d . . . . .
C19 C 0.3361(3) 0.5554(3) 0.29154(11) 0.0246(7) Uani 1 1 d . . . . .
C20 C 0.4396(4) 0.5167(3) 0.26758(10) 0.0251(7) Uani 1 1 d . . . . .
H20 H 0.422322 0.468448 0.244312 0.030 Uiso 1 1 calc R . . . .
C21 C 0.5666(3) 0.5450(3) 0.27597(10) 0.0245(7) Uani 1 1 d . . . . .
C22 C 0.5907(3) 0.6165(3) 0.31012(10) 0.0230(7) Uani 1 1 d . . . . .
H22 H 0.676751 0.636694 0.316694 0.028 Uiso 1 1 calc R . . . .
C23 C 0.1975(3) 0.5207(3) 0.28114(11) 0.0280(7) Uani 1 1 d . . . . .
C24 C 0.1138(4) 0.6267(4) 0.27291(14) 0.0386(9) Uani 1 1 d . . . . .
H24A H 0.110787 0.673751 0.298310 0.058 Uiso 1 1 calc GR . . . .
H24B H 0.026559 0.602804 0.265413 0.058 Uiso 1 1 calc GR . . . .
H24C H 0.150783 0.670911 0.249783 0.058 Uiso 1 1 calc GR . . . .
C25 C 0.1418(4) 0.4512(3) 0.31807(12) 0.0316(8) Uani 1 1 d . . . . .
H25A H 0.193024 0.382083 0.322080 0.047 Uiso 1 1 calc GR . . . .
H25B H 0.052749 0.430320 0.311820 0.047 Uiso 1 1 calc GR . . . .
H25C H 0.144425 0.497167 0.343743 0.047 Uiso 1 1 calc GR . . . .
C26 C 0.1900(4) 0.4454(4) 0.24192(13) 0.0370(9) Uani 1 1 d . . . . .
H26A H 0.226638 0.486277 0.217903 0.055 Uiso 1 1 calc GR . . . .
H26B H 0.100095 0.426677 0.236073 0.055 Uiso 1 1 calc GR . . . .
H26C H 0.238625 0.375191 0.246709 0.055 Uiso 1 1 calc GR . . . .
C27 C 0.6791(3) 0.5024(3) 0.24913(11) 0.0272(7) Uani 1 1 d . . . . .
C28 C 0.7494(4) 0.6058(3) 0.23055(12) 0.0347(9) Uani 1 1 d . . . . .
H28A H 0.691184 0.647382 0.211856 0.052 Uiso 1 1 calc GR . . . .
H28B H 0.824403 0.579869 0.214603 0.052 Uiso 1 1 calc GR . . . .
H28C H 0.777448 0.656033 0.253340 0.052 Uiso 1 1 calc GR . . . .
C29 C 0.7724(4) 0.4345(4) 0.27621(13) 0.0375(9) Uani 1 1 d . . . . .
H29A H 0.803971 0.482612 0.299154 0.056 Uiso 1 1 calc GR . . . .
H29B H 0.845021 0.409307 0.258974 0.056 Uiso 1 1 calc GR . . . .
H29C H 0.728292 0.368068 0.287920 0.056 Uiso 1 1 calc GR . . . .
C30 C 0.6351(4) 0.4265(4) 0.21250(13) 0.0382(9) Uani 1 1 d . . . . .
H30A H 0.586198 0.361810 0.223521 0.057 Uiso 1 1 calc GR . . . .
H30B H 0.710424 0.398518 0.197200 0.057 Uiso 1 1 calc GR . . . .
H30C H 0.580664 0.470794 0.193439 0.057 Uiso 1 1 calc GR . . . .
C31 C 0.4635(3) 0.6132(3) 0.42694(10) 0.0225(7) Uani 1 1 d . . . . .
H31 H 0.477655 0.557970 0.403500 0.027 Uiso 1 1 calc R . . . .
C32 C 0.3392(3) 0.5788(3) 0.44873(10) 0.0260(7) Uani 1 1 d . . . . .
C33 C 0.2305(5) 0.4247(4) 0.48185(18) 0.0531(13) Uani 1 1 d D . . . .
H33A H 0.151182 0.440408 0.465702 0.064 Uiso 0.583(13) 1 calc R . P A 1
H33B H 0.222261 0.459314 0.510063 0.064 Uiso 0.583(13) 1 calc R . P A 1
H33C H 0.258484 0.358879 0.498978 0.064 Uiso 0.417(13) 1 calc R . P A 2
H33D H 0.199424 0.483837 0.501509 0.064 Uiso 0.417(13) 1 calc R . P A 2
C34 C 0.2537(9) 0.2959(6) 0.4853(2) 0.045(2) Uani 0.583(13) 1 d D . P A 1
H34A H 0.268218 0.264111 0.457277 0.068 Uiso 0.583(13) 1 calc GR . P A 1
H34B H 0.178450 0.259518 0.498048 0.068 Uiso 0.583(13) 1 calc GR . P A 1
H34C H 0.329336 0.281864 0.502934 0.068 Uiso 0.583(13) 1 calc GR . P A 1
C35 C 0.5774(3) 0.5990(3) 0.45800(11) 0.0259(7) Uani 1 1 d . . . . .
H35A H 0.566127 0.653523 0.481404 0.031 Uiso 1 1 calc R . . . .
H35B H 0.574089 0.521331 0.470018 0.031 Uiso 1 1 calc R . . . .
C36 C 0.7084(3) 0.6173(3) 0.43877(10) 0.0234(7) Uani 1 1 d . . . . .
C37 C 0.7525(4) 0.5486(3) 0.40642(13) 0.0328(8) Uani 1 1 d . . . . .
H37 H 0.699018 0.489695 0.395862 0.039 Uiso 1 1 calc R . . . .
C38 C 0.8742(4) 0.5646(4) 0.38919(13) 0.0375(9) Uani 1 1 d . . . . .
H38 H 0.902469 0.517374 0.366808 0.045 Uiso 1 1 calc R . . . .
C39 C 0.9535(4) 0.6486(4) 0.40447(12) 0.0354(9) Uani 1 1 d . . . . .
H39 H 1.037102 0.658770 0.393128 0.043 Uiso 1 1 calc R . . . .
C40 C 0.9104(4) 0.7176(4) 0.43634(13) 0.0349(9) Uani 1 1 d . . . . .
H40 H 0.964437 0.776150 0.446834 0.042 Uiso 1 1 calc R . . . .
C41 C 0.7889(4) 0.7028(3) 0.45338(11) 0.0283(7) Uani 1 1 d . . . . .
H41 H 0.760571 0.751687 0.475272 0.034 Uiso 1 1 calc R . . . .
C34A C 0.1314(13) 0.3914(12) 0.4583(4) 0.064(4) Uani 0.417(13) 1 d D . P A 2
H34D H 0.101013 0.455693 0.441357 0.096 Uiso 0.417(13) 1 calc GR . P A 2
H34E H 0.061814 0.364603 0.476454 0.096 Uiso 0.417(13) 1 calc GR . P A 2
H34F H 0.158744 0.329583 0.439644 0.096 Uiso 0.417(13) 1 calc GR . P A 2


_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
O1 C3 1.370(4) . ?
N1 C1 1.481(4) . ?
N1 C16 1.481(4) . ?
N1 C31 1.471(4) . ?
C1 C2 1.510(5) . ?
O2 C18 1.373(4) . ?
C2 C3 1.398(5) . ?
C2 C7 1.391(5) . ?
O3 C32 1.208(5) . ?
C3 C4 1.413(5) . ?
O4 C32 1.334(4) . ?
O4 C33 1.458(5) . ?
C4 C5 1.404(5) . ?
C4 C8 1.537(5) . ?
C5 C6 1.397(5) . ?
C6 C7 1.394(5) . ?
C6 C12 1.523(5) . ?
C8 C9 1.538(5) . ?
C8 C10 1.539(5) . ?
C8 C11 1.549(5) . ?
C12 C13 1.514(5) . ?
C12 C14 1.559(6) . ?
C12 C15 1.527(7) . ?
C16 C17 1.516(4) . ?
C17 C18 1.403(5) . ?
C17 C22 1.392(5) . ?
C18 C19 1.407(5) . ?
C19 C20 1.397(5) . ?
C19 C23 1.536(5) . ?
C20 C21 1.388(5) . ?
C21 C22 1.397(5) . ?
C21 C27 1.534(5) . ?
C23 C24 1.544(5) . ?
C23 C25 1.544(5) . ?
C23 C26 1.532(5) . ?
C27 C28 1.537(5) . ?
C27 C29 1.525(6) . ?
C27 C30 1.538(5) . ?
C31 C32 1.523(5) . ?
C31 C35 1.553(5) . ?
C33 C34 1.537(9) . ?
C33 C34A 1.334(12) . ?
C35 C36 1.510(5) . ?
C36 C37 1.387(5) . ?
C36 C41 1.389(5) . ?
C37 C38 1.393(6) . ?
C38 C39 1.376(6) . ?
C39 C40 1.374(6) . ?
C40 C41 1.386(6) . ?

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
C1 N1 C16 111.5(2) . . ?
C31 N1 C1 114.2(3) . . ?
C31 N1 C16 114.1(3) . . ?
N1 C1 C2 111.4(3) . . ?
C3 C2 C1 121.3(3) . . ?
C7 C2 C1 119.3(3) . . ?
C7 C2 C3 119.3(3) . . ?
O1 C3 C2 120.7(3) . . ?
O1 C3 C4 118.4(3) . . ?
C2 C3 C4 120.9(3) . . ?
C32 O4 C33 117.1(3) . . ?
C3 C4 C8 121.6(3) . . ?
C5 C4 C3 116.9(3) . . ?
C5 C4 C8 121.5(3) . . ?
C6 C5 C4 123.9(3) . . ?
C5 C6 C12 124.0(3) . . ?
C7 C6 C5 116.6(3) . . ?
C7 C6 C12 119.4(3) . . ?
C2 C7 C6 122.4(3) . . ?
C4 C8 C9 110.3(3) . . ?
C4 C8 C10 112.2(3) . . ?
C4 C8 C11 109.8(3) . . ?
C9 C8 C10 107.7(3) . . ?
C9 C8 C11 109.8(3) . . ?
C10 C8 C11 106.9(3) . . ?
C6 C12 C14 108.7(3) . . ?
C6 C12 C15 109.2(3) . . ?
C13 C12 C6 113.1(3) . . ?
C13 C12 C14 107.5(3) . . ?
C13 C12 C15 109.9(4) . . ?
C15 C12 C14 108.2(4) . . ?
N1 C16 C17 113.1(3) . . ?
C18 C17 C16 121.1(3) . . ?
C22 C17 C16 119.0(3) . . ?
C22 C17 C18 119.7(3) . . ?
O2 C18 C17 119.8(3) . . ?
O2 C18 C19 119.7(3) . . ?
C17 C18 C19 120.6(3) . . ?
C18 C19 C23 121.2(3) . . ?
C20 C19 C18 117.4(3) . . ?
C20 C19 C23 121.4(3) . . ?
C21 C20 C19 123.5(3) . . ?
C20 C21 C22 117.7(3) . . ?
C20 C21 C27 122.8(3) . . ?
C22 C21 C27 119.5(3) . . ?
C17 C22 C21 121.2(3) . . ?
C19 C23 C24 110.7(3) . . ?
C19 C23 C25 109.2(3) . . ?
C24 C23 C25 110.1(3) . . ?
C26 C23 C19 112.1(3) . . ?
C26 C23 C24 107.4(3) . . ?
C26 C23 C25 107.2(3) . . ?
C21 C27 C28 108.7(3) . . ?
C21 C27 C30 112.6(3) . . ?
C28 C27 C30 108.0(3) . . ?
C29 C27 C21 110.0(3) . . ?
C29 C27 C28 109.1(3) . . ?
C29 C27 C30 108.3(3) . . ?
N1 C31 C32 108.6(3) . . ?
N1 C31 C35 117.4(3) . . ?
C32 C31 C35 109.3(3) . . ?
O3 C32 O4 123.5(3) . . ?
O3 C32 C31 125.7(3) . . ?
O4 C32 C31 110.8(3) . . ?
O4 C33 C34 105.3(5) . . ?
C34A C33 O4 117.2(7) . . ?
C36 C35 C31 114.6(3) . . ?
C37 C36 C35 121.1(3) . . ?
C37 C36 C41 118.0(3) . . ?
C41 C36 C35 120.9(3) . . ?
C36 C37 C38 121.0(3) . . ?
C39 C38 C37 120.2(4) . . ?
C40 C39 C38 119.2(4) . . ?
C39 C40 C41 120.9(4) . . ?
C40 C41 C36 120.7(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_cu_8v00512_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2070847'
loop_
_audit_author_name
_audit_author_address
'Georgina M. Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-03-16 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2021-03-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H55 N O4'
_chemical_formula_sum            'C35 H55 N O4'
_chemical_formula_weight         553.80
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.08240(10)
_cell_length_b                   11.7694(2)
_cell_length_c                   31.5208(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3369.40(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.127
_cell_measurement_theta_min      4.010
_shelx_estimated_absorpt_T_max   0.938
_shelx_estimated_absorpt_T_min   0.812
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0764 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.9305.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            47117
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.121
_diffrn_reflns_theta_min         2.804
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6552
_reflns_number_total             6637
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 
;
 Flack x determined using 2833 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6637
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0262
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+0.5417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0696
_refine_special_details          ?
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C25(H25), C27(H27)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.48002(11) 0.53897(8) 0.45168(3) 0.0201(2) Uani 1 1 d . . . . .
H1 H 0.534742 0.481803 0.449241 0.030 Uiso 1 1 calc R U . . .
O2 O 0.43330(11) 0.35979(9) 0.36270(3) 0.0202(2) Uani 1 1 d . . . . .
H2 H 0.495432 0.389519 0.379018 0.030 Uiso 1 1 calc R U . . .
O3 O 0.60082(12) 0.32279(9) 0.46430(3) 0.0272(2) Uani 1 1 d . . . . .
O4 O 0.75671(12) 0.17509(9) 0.45984(3) 0.0261(2) Uani 1 1 d . . . . .
N1 N 0.70807(12) 0.41793(9) 0.39141(3) 0.0153(2) Uani 1 1 d . . . . .
C1 C 0.76738(16) 0.30664(11) 0.40423(4) 0.0183(3) Uani 1 1 d . . . . .
H1A H 0.733876 0.250462 0.382469 0.022 Uiso 1 1 calc R U . . .
C2 C 0.69731(17) 0.27170(12) 0.44607(4) 0.0202(3) Uani 1 1 d . . . . .
C3 C 0.69701(19) 0.12671(14) 0.49878(5) 0.0279(3) Uani 1 1 d . . . . .
H3A H 0.669703 0.188451 0.518607 0.034 Uiso 1 1 calc R U . . .
H3B H 0.772447 0.078737 0.512680 0.034 Uiso 1 1 calc R U . . .
C4 C 0.5640(2) 0.05648(15) 0.48861(5) 0.0338(4) Uani 1 1 d . . . . .
H4A H 0.590060 -0.001305 0.467525 0.051 Uiso 1 1 calc R U . . .
H4B H 0.486403 0.105563 0.477187 0.051 Uiso 1 1 calc R U . . .
H4C H 0.528600 0.019246 0.514484 0.051 Uiso 1 1 calc R U . . .
C5 C 0.93594(17) 0.29845(13) 0.40612(5) 0.0252(3) Uani 1 1 d . . . . .
H5A H 0.977880 0.325997 0.379390 0.038 Uiso 1 1 calc R U . . .
H5B H 0.964926 0.219125 0.410557 0.038 Uiso 1 1 calc R U . . .
H5C H 0.972609 0.344988 0.429640 0.038 Uiso 1 1 calc R U . . .
C6 C 0.77062(15) 0.51285(11) 0.41641(4) 0.0163(3) Uani 1 1 d . . . . .
H6A H 0.872738 0.527509 0.406886 0.020 Uiso 1 1 calc R U . . .
H6B H 0.774132 0.490959 0.446718 0.020 Uiso 1 1 calc R U . . .
C7 C 0.68118(15) 0.61992(11) 0.41172(4) 0.0156(3) Uani 1 1 d . . . . .
C8 C 0.54044(15) 0.62864(12) 0.42991(4) 0.0157(3) Uani 1 1 d . . . . .
C9 C 0.46010(15) 0.73036(12) 0.42712(4) 0.0159(3) Uani 1 1 d . . . . .
C10 C 0.52409(15) 0.81976(11) 0.40409(4) 0.0161(3) Uani 1 1 d . . . . .
H10 H 0.470155 0.888522 0.401316 0.019 Uiso 1 1 calc R U . . .
C11 C 0.66263(15) 0.81317(11) 0.38505(4) 0.0161(3) Uani 1 1 d . . . . .
C12 C 0.73951(15) 0.71150(11) 0.38986(4) 0.0158(3) Uani 1 1 d . . . . .
H12 H 0.834913 0.704821 0.377753 0.019 Uiso 1 1 calc R U . . .
C13 C 0.30887(15) 0.74338(12) 0.44889(4) 0.0182(3) Uani 1 1 d . . . . .
C14 C 0.19777(15) 0.65774(12) 0.43051(4) 0.0205(3) Uani 1 1 d . . . . .
H14A H 0.183341 0.673102 0.400237 0.031 Uiso 1 1 calc R U . . .
H14B H 0.103557 0.665191 0.445408 0.031 Uiso 1 1 calc R U . . .
H14C H 0.235685 0.580406 0.434182 0.031 Uiso 1 1 calc R U . . .
C15 C 0.32506(17) 0.72460(14) 0.49715(5) 0.0235(3) Uani 1 1 d . . . . .
H15A H 0.364730 0.648472 0.502429 0.035 Uiso 1 1 calc R U . . .
H15B H 0.228473 0.731758 0.510745 0.035 Uiso 1 1 calc R U . . .
H15C H 0.392254 0.781658 0.508889 0.035 Uiso 1 1 calc R U . . .
C16 C 0.24375(16) 0.86294(13) 0.44278(5) 0.0244(3) Uani 1 1 d . . . . .
H16A H 0.310911 0.919501 0.454872 0.037 Uiso 1 1 calc R U . . .
H16B H 0.148252 0.867582 0.457147 0.037 Uiso 1 1 calc R U . . .
H16C H 0.230623 0.877901 0.412431 0.037 Uiso 1 1 calc R U . . .
C17 C 0.73317(15) 0.91039(11) 0.35974(4) 0.0191(3) Uani 1 1 d . . . . .
C18 C 0.77510(19) 0.86818(14) 0.31536(5) 0.0284(3) Uani 1 1 d . . . . .
H18A H 0.842525 0.803516 0.317868 0.043 Uiso 1 1 calc R U . . .
H18B H 0.823487 0.929588 0.299656 0.043 Uiso 1 1 calc R U . . .
H18C H 0.686122 0.844440 0.300170 0.043 Uiso 1 1 calc R U . . .
C19 C 0.63032(17) 1.01227(13) 0.35464(5) 0.0250(3) Uani 1 1 d . . . . .
H19A H 0.540276 0.988281 0.340037 0.038 Uiso 1 1 calc R U . . .
H19B H 0.679628 1.071307 0.337944 0.038 Uiso 1 1 calc R U . . .
H19C H 0.605096 1.042544 0.382678 0.038 Uiso 1 1 calc R U . . .
C20 C 0.87357(17) 0.95013(14) 0.38299(5) 0.0280(3) Uani 1 1 d . . . . .
H20A H 0.847286 0.978553 0.411219 0.042 Uiso 1 1 calc R U . . .
H20B H 0.920732 1.010969 0.366685 0.042 Uiso 1 1 calc R U . . .
H20C H 0.941849 0.886109 0.385846 0.042 Uiso 1 1 calc R U . . .
C21 C 0.72551(15) 0.43949(11) 0.34543(4) 0.0164(3) Uani 1 1 d . . . . .
H21A H 0.831701 0.439162 0.338341 0.020 Uiso 1 1 calc R U . . .
H21B H 0.686445 0.515978 0.338787 0.020 Uiso 1 1 calc R U . . .
C22 C 0.64752(15) 0.35280(11) 0.31804(4) 0.0158(3) Uani 1 1 d . . . . .
C23 C 0.50354(15) 0.31771(11) 0.32748(4) 0.0162(3) Uani 1 1 d . . . . .
C24 C 0.42955(15) 0.24093(11) 0.30096(4) 0.0165(3) Uani 1 1 d . . . . .
C25 C 0.50352(15) 0.20415(11) 0.26451(4) 0.0168(3) Uani 1 1 d . . . . .
H25 H 0.453880 0.153247 0.246005 0.020 Uiso 1 1 calc R U . . .
C26 C 0.64574(15) 0.23791(11) 0.25382(4) 0.0158(3) Uani 1 1 d . . . . .
C27 C 0.71703(14) 0.31193(11) 0.28174(4) 0.0155(3) Uani 1 1 d . . . . .
H27 H 0.815185 0.334890 0.275821 0.019 Uiso 1 1 calc R U . . .
C28 C 0.27084(15) 0.20180(12) 0.31022(4) 0.0192(3) Uani 1 1 d . . . . .
C29 C 0.25790(16) 0.14935(13) 0.35489(5) 0.0246(3) Uani 1 1 d . . . . .
H29A H 0.323518 0.083499 0.357033 0.037 Uiso 1 1 calc R U . . .
H29B H 0.156082 0.125184 0.359831 0.037 Uiso 1 1 calc R U . . .
H29C H 0.285887 0.206032 0.376187 0.037 Uiso 1 1 calc R U . . .
C30 C 0.21987(16) 0.11095(13) 0.27840(5) 0.0248(3) Uani 1 1 d . . . . .
H30A H 0.218265 0.143473 0.249780 0.037 Uiso 1 1 calc R U . . .
H30B H 0.120802 0.085016 0.286010 0.037 Uiso 1 1 calc R U . . .
H30C H 0.288067 0.046450 0.279119 0.037 Uiso 1 1 calc R U . . .
C31 C 0.16683(16) 0.30440(13) 0.30628(5) 0.0230(3) Uani 1 1 d . . . . .
H31A H 0.193707 0.361806 0.327428 0.034 Uiso 1 1 calc R U . . .
H31B H 0.065156 0.279712 0.311116 0.034 Uiso 1 1 calc R U . . .
H31C H 0.175353 0.337062 0.277785 0.034 Uiso 1 1 calc R U . . .
C32 C 0.72271(15) 0.19781(11) 0.21315(4) 0.0175(3) Uani 1 1 d . . . . .
C33 C 0.86546(17) 0.13560(14) 0.22460(5) 0.0256(3) Uani 1 1 d . . . . .
H33A H 0.930333 0.187004 0.240372 0.038 Uiso 1 1 calc R U . . .
H33B H 0.914924 0.110755 0.198570 0.038 Uiso 1 1 calc R U . . .
H33C H 0.842424 0.069260 0.242173 0.038 Uiso 1 1 calc R U . . .
C34 C 0.76154(19) 0.30226(13) 0.18599(4) 0.0247(3) Uani 1 1 d . . . . .
H34A H 0.671116 0.342939 0.178440 0.037 Uiso 1 1 calc R U . . .
H34B H 0.811852 0.277546 0.160081 0.037 Uiso 1 1 calc R U . . .
H34C H 0.826382 0.352800 0.202159 0.037 Uiso 1 1 calc R U . . .
C35 C 0.62588(18) 0.11810(13) 0.18676(5) 0.0239(3) Uani 1 1 d . . . . .
H35A H 0.597731 0.052269 0.203984 0.036 Uiso 1 1 calc R U . . .
H35B H 0.680808 0.092354 0.161786 0.036 Uiso 1 1 calc R U . . .
H35C H 0.537144 0.158669 0.177629 0.036 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.8400 . ?
O1 C8 1.3733(16) . ?
O2 H2 0.8400 . ?
O2 C23 1.3727(16) . ?
O3 C2 1.2082(18) . ?
O4 C2 1.3313(17) . ?
O4 C3 1.4577(17) . ?
N1 C1 1.4728(16) . ?
N1 C6 1.4804(17) . ?
N1 C21 1.4798(16) . ?
C1 H1A 1.0000 . ?
C1 C2 1.5212(19) . ?
C1 C5 1.535(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.498(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.5065(18) . ?
C7 C8 1.4047(19) . ?
C7 C12 1.3848(19) . ?
C8 C9 1.4048(19) . ?
C9 C10 1.4042(19) . ?
C9 C13 1.5431(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.3962(19) . ?
C11 C12 1.3937(19) . ?
C11 C17 1.5351(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.5394(19) . ?
C13 C15 1.5440(19) . ?
C13 C16 1.5385(19) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.533(2) . ?
C17 C19 1.5284(19) . ?
C17 C20 1.544(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.5127(18) . ?
C22 C23 1.4033(19) . ?
C22 C27 1.3926(18) . ?
C23 C24 1.4025(19) . ?
C24 C25 1.3996(19) . ?
C24 C28 1.5411(18) . ?
C25 H25 0.9500 . ?
C25 C26 1.3929(19) . ?
C26 C27 1.3974(19) . ?
C26 C32 1.5346(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.5419(19) . ?
C28 C30 1.537(2) . ?
C28 C31 1.5382(19) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.5320(19) . ?
C32 C34 1.5388(19) . ?
C32 C35 1.5314(19) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

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
C8 O1 H1 109.5 . . ?
C23 O2 H2 109.5 . . ?
C2 O4 C3 117.22(12) . . ?
C1 N1 C6 112.63(10) . . ?
C1 N1 C21 112.46(10) . . ?
C21 N1 C6 110.54(10) . . ?
N1 C1 H1A 106.8 . . ?
N1 C1 C2 108.98(11) . . ?
N1 C1 C5 115.55(12) . . ?
C2 C1 H1A 106.8 . . ?
C2 C1 C5 111.49(12) . . ?
C5 C1 H1A 106.8 . . ?
O3 C2 O4 124.33(13) . . ?
O3 C2 C1 125.55(13) . . ?
O4 C2 C1 110.12(12) . . ?
O4 C3 H3A 109.8 . . ?
O4 C3 H3B 109.8 . . ?
O4 C3 C4 109.59(13) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.2 . . ?
N1 C6 H6B 109.2 . . ?
N1 C6 C7 111.84(11) . . ?
H6A C6 H6B 107.9 . . ?
C7 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C8 C7 C6 120.79(12) . . ?
C12 C7 C6 119.58(12) . . ?
C12 C7 C8 119.63(12) . . ?
O1 C8 C7 120.75(12) . . ?
O1 C8 C9 118.60(11) . . ?
C7 C8 C9 120.62(12) . . ?
C8 C9 C13 121.27(12) . . ?
C10 C9 C8 117.13(12) . . ?
C10 C9 C13 121.60(12) . . ?
C9 C10 H10 118.2 . . ?
C11 C10 C9 123.61(12) . . ?
C11 C10 H10 118.2 . . ?
C10 C11 C17 123.92(12) . . ?
C12 C11 C10 116.91(12) . . ?
C12 C11 C17 119.17(12) . . ?
C7 C12 C11 122.05(12) . . ?
C7 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C9 C13 C15 109.83(11) . . ?
C14 C13 C9 110.55(11) . . ?
C14 C13 C15 109.85(11) . . ?
C16 C13 C9 112.17(11) . . ?
C16 C13 C14 107.44(11) . . ?
C16 C13 C15 106.91(12) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 C20 108.89(12) . . ?
C18 C17 C11 109.67(11) . . ?
C18 C17 C20 109.05(13) . . ?
C19 C17 C11 112.60(11) . . ?
C19 C17 C18 108.08(12) . . ?
C19 C17 C20 108.49(12) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 H21A 108.9 . . ?
N1 C21 H21B 108.9 . . ?
N1 C21 C22 113.15(11) . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C23 C22 C21 120.92(12) . . ?
C27 C22 C21 119.32(12) . . ?
C27 C22 C23 119.67(12) . . ?
O2 C23 C22 119.89(12) . . ?
O2 C23 C24 119.45(12) . . ?
C24 C23 C22 120.65(12) . . ?
C23 C24 C28 121.87(12) . . ?
C25 C24 C23 117.29(12) . . ?
C25 C24 C28 120.79(12) . . ?
C24 C25 H25 118.1 . . ?
C26 C25 C24 123.75(13) . . ?
C26 C25 H25 118.1 . . ?
C25 C26 C27 117.07(12) . . ?
C25 C26 C32 122.48(12) . . ?
C27 C26 C32 120.45(12) . . ?
C22 C27 C26 121.52(12) . . ?
C22 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C24 C28 C29 111.33(11) . . ?
C30 C28 C24 111.47(12) . . ?
C30 C28 C29 107.12(12) . . ?
C30 C28 C31 107.97(11) . . ?
C31 C28 C24 108.94(11) . . ?
C31 C28 C29 109.95(12) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C26 C32 C34 108.87(11) . . ?
C33 C32 C26 109.61(11) . . ?
C33 C32 C34 108.60(12) . . ?
C35 C32 C26 112.36(11) . . ?
C35 C32 C33 108.73(12) . . ?
C35 C32 C34 108.60(11) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O3 0.84 2.02 2.7992(14) 153.6 . yes
O2 H2 N1 0.84 2.00 2.7414(15) 147.0 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C8 C9 C10 -179.07(11) . . . . ?
O1 C8 C9 C13 1.61(18) . . . . ?
O2 C23 C24 C25 177.38(11) . . . . ?
O2 C23 C24 C28 -0.13(19) . . . . ?
N1 C1 C2 O3 5.0(2) . . . . ?
N1 C1 C2 O4 -175.67(11) . . . . ?
N1 C6 C7 C8 70.42(15) . . . . ?
N1 C6 C7 C12 -110.72(13) . . . . ?
N1 C21 C22 C23 44.77(16) . . . . ?
N1 C21 C22 C27 -138.61(12) . . . . ?
C1 N1 C6 C7 -164.32(11) . . . . ?
C1 N1 C21 C22 60.21(15) . . . . ?
C2 O4 C3 C4 84.62(16) . . . . ?
C3 O4 C2 O3 2.1(2) . . . . ?
C3 O4 C2 C1 -177.24(12) . . . . ?
C5 C1 C2 O3 133.70(16) . . . . ?
C5 C1 C2 O4 -46.94(16) . . . . ?
C6 N1 C1 C2 75.25(14) . . . . ?
C6 N1 C1 C5 -51.18(15) . . . . ?
C6 N1 C21 C22 -172.97(11) . . . . ?
C6 C7 C8 O1 -1.26(18) . . . . ?
C6 C7 C8 C9 177.11(12) . . . . ?
C6 C7 C12 C11 -179.08(12) . . . . ?
C7 C8 C9 C10 2.53(18) . . . . ?
C7 C8 C9 C13 -176.80(12) . . . . ?
C8 C7 C12 C11 -0.20(19) . . . . ?
C8 C9 C10 C11 -1.49(19) . . . . ?
C8 C9 C13 C14 -61.97(16) . . . . ?
C8 C9 C13 C15 59.40(16) . . . . ?
C8 C9 C13 C16 178.14(12) . . . . ?
C9 C10 C11 C12 -0.35(19) . . . . ?
C9 C10 C11 C17 179.84(12) . . . . ?
C10 C9 C13 C14 118.74(13) . . . . ?
C10 C9 C13 C15 -119.89(14) . . . . ?
C10 C9 C13 C16 -1.16(18) . . . . ?
C10 C11 C12 C7 1.23(19) . . . . ?
C10 C11 C17 C18 -124.86(14) . . . . ?
C10 C11 C17 C19 -4.48(19) . . . . ?
C10 C11 C17 C20 115.89(14) . . . . ?
C12 C7 C8 O1 179.88(12) . . . . ?
C12 C7 C8 C9 -1.75(18) . . . . ?
C12 C11 C17 C18 55.34(16) . . . . ?
C12 C11 C17 C19 175.72(12) . . . . ?
C12 C11 C17 C20 -63.92(16) . . . . ?
C13 C9 C10 C11 177.83(12) . . . . ?
C17 C11 C12 C7 -178.95(12) . . . . ?
C21 N1 C1 C2 -159.05(11) . . . . ?
C21 N1 C1 C5 74.52(15) . . . . ?
C21 N1 C6 C7 68.95(14) . . . . ?
C21 C22 C23 O2 -1.89(18) . . . . ?
C21 C22 C23 C24 177.30(12) . . . . ?
C21 C22 C27 C26 -175.47(12) . . . . ?
C22 C23 C24 C25 -1.81(19) . . . . ?
C22 C23 C24 C28 -179.33(11) . . . . ?
C23 C22 C27 C26 1.19(19) . . . . ?
C23 C24 C25 C26 1.17(19) . . . . ?
C23 C24 C28 C29 -56.05(16) . . . . ?
C23 C24 C28 C30 -175.60(12) . . . . ?
C23 C24 C28 C31 65.37(16) . . . . ?
C24 C25 C26 C27 0.61(19) . . . . ?
C24 C25 C26 C32 -178.79(12) . . . . ?
C25 C24 C28 C29 126.52(13) . . . . ?
C25 C24 C28 C30 6.97(17) . . . . ?
C25 C24 C28 C31 -112.07(14) . . . . ?
C25 C26 C27 C22 -1.81(19) . . . . ?
C25 C26 C32 C33 -121.16(14) . . . . ?
C25 C26 C32 C34 120.18(14) . . . . ?
C25 C26 C32 C35 -0.15(18) . . . . ?
C27 C22 C23 O2 -178.50(12) . . . . ?
C27 C22 C23 C24 0.69(19) . . . . ?
C27 C26 C32 C33 59.46(16) . . . . ?
C27 C26 C32 C34 -59.20(16) . . . . ?
C27 C26 C32 C35 -179.53(12) . . . . ?
C28 C24 C25 C26 178.71(12) . . . . ?
C32 C26 C27 C22 177.60(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_8v00160_0m
_database_code_depnum_ccdc_archive 'CCDC 2070851'
loop_
_audit_author_name
_audit_author_address
'Georgina M. Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-03-16 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2021-03-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H31 N O4'
_chemical_formula_sum            'C23 H31 N O4'
_chemical_formula_weight         385.49
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5479(2)
_cell_length_b                   14.5535(3)
_cell_length_c                   15.4442(3)
_cell_angle_alpha                70.3610(10)
_cell_angle_beta                 70.5070(10)
_cell_angle_gamma                76.5600(10)
_cell_volume                     2085.52(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3876
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      50.90
_cell_measurement_theta_min      3.79
_shelx_estimated_absorpt_T_max   0.901
_shelx_estimated_absorpt_T_min   0.815
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.8374.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24899
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.563
_diffrn_reflns_theta_min         3.164
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5755
_reflns_number_total             8049
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0494
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0729P)²+0.0723P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1405
_refine_special_details          ?
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C2'(H2')
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C7(H7a,H7b), C16(H16a,H16b), C5'(H5'a,H5'b), C7'(H7'a,H7'b),
 C16'(H16c,H16d)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C20(H20), C22(H22), C11'(H11'), C13'(H13'), C20'(H20'),
 C22'(H22')
2.d Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C6(H6a,H6b,H6c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c),
 C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C3'(H3'a,H3'b,H3'c), C6'(H6'a,H6'b,
 H6'c), C14'(H14d,H14e,H14f), C15'(H15d,H15e,H15f), C23'(H23d,H23e,H23f),
 C24'(H24d,H24e,H24f)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2a), O1'(H1'), O2'(H2'a)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.43370(14) 0.53904(10) 0.14604(11) 0.0383(3) Uani 1 1 d . . . . .
N1 N 0.59840(15) 0.64711(11) 0.16367(11) 0.0281(3) Uani 1 1 d . . . . .
O1 O 0.68828(13) 0.69156(11) -0.03710(10) 0.0338(3) Uani 1 1 d . . . . .
H1 H 0.6285 0.6905 0.0151 0.051 Uiso 1 1 calc GR . . . .
C2 C 0.62866(18) 0.53930(14) 0.19540(14) 0.0297(4) Uani 1 1 d . . . . .
H2 H 0.7136 0.5215 0.1472 0.036 Uiso 1 1 calc R . . . .
O2 O 0.37806(14) 0.74057(11) 0.06407(11) 0.0383(3) Uani 1 1 d . . . . .
H2A H 0.4075 0.6854 0.0961 0.057 Uiso 1 1 calc GR . . . .
C3 C 0.6586(2) 0.49445(16) 0.29246(15) 0.0380(5) Uani 1 1 d . . . . .
H3A H 0.5777 0.5084 0.3430 0.057 Uiso 1 1 calc GR . . . .
H3B H 0.7339 0.5232 0.2926 0.057 Uiso 1 1 calc GR . . . .
H3C H 0.6836 0.4231 0.3040 0.057 Uiso 1 1 calc GR . . . .
O4 O 0.52995(14) 0.39780(10) 0.22876(11) 0.0399(4) Uani 1 1 d . . . . .
C4 C 0.51911(19) 0.49393(15) 0.18699(15) 0.0329(4) Uani 1 1 d . . . . .
C5 C 0.4300(2) 0.34525(16) 0.2252(2) 0.0481(6) Uani 1 1 d . . . . .
H5A H 0.4389 0.3499 0.1581 0.058 Uiso 1 1 calc R . . . .
H5B H 0.3369 0.3741 0.2539 0.058 Uiso 1 1 calc R . . . .
C6 C 0.4571(3) 0.24098(18) 0.2802(2) 0.0663(8) Uani 1 1 d . . . . .
H6A H 0.5475 0.2122 0.2490 0.100 Uiso 1 1 calc GR . . . .
H6B H 0.3887 0.2041 0.2825 0.100 Uiso 1 1 calc GR . . . .
H6C H 0.4531 0.2377 0.3455 0.100 Uiso 1 1 calc GR . . . .
C7 C 0.71867(18) 0.69542(14) 0.14145(14) 0.0290(4) Uani 1 1 d . . . . .
H7A H 0.7483 0.6784 0.2000 0.035 Uiso 1 1 calc R . . . .
H7B H 0.6934 0.7677 0.1213 0.035 Uiso 1 1 calc R . . . .
C8 C 0.83521(18) 0.66518(13) 0.06331(13) 0.0260(4) Uani 1 1 d . . . . .
C9 C 0.81475(18) 0.66589(13) -0.02151(13) 0.0272(4) Uani 1 1 d . . . . .
C10 C 0.92271(18) 0.64123(13) -0.09576(13) 0.0271(4) Uani 1 1 d . . . . .
C11 C 1.05183(19) 0.61913(13) -0.08331(14) 0.0291(4) Uani 1 1 d . . . . .
H11 H 1.1264 0.6048 -0.1343 0.035 Uiso 1 1 calc R . . . .
C12 C 1.07754(18) 0.61690(13) -0.00010(14) 0.0281(4) Uani 1 1 d . . . . .
C13 C 0.96658(18) 0.63829(13) 0.07330(14) 0.0275(4) Uani 1 1 d . . . . .
H13 H 0.9807 0.6345 0.1321 0.033 Uiso 1 1 calc R . . . .
C14 C 0.8982(2) 0.63943(16) -0.18525(14) 0.0354(5) Uani 1 1 d . . . . .
H14A H 0.9841 0.6180 -0.2280 0.053 Uiso 1 1 calc GR . . . .
H14B H 0.8612 0.7056 -0.2175 0.053 Uiso 1 1 calc GR . . . .
H14C H 0.8335 0.5935 -0.1688 0.053 Uiso 1 1 calc GR . . . .
C15 C 1.21962(19) 0.59323(15) 0.00939(15) 0.0338(4) Uani 1 1 d . . . . .
H15A H 1.2544 0.5245 0.0102 0.051 Uiso 1 1 calc GR . . . .
H15B H 1.2192 0.6033 0.0691 0.051 Uiso 1 1 calc GR . . . .
H15C H 1.2780 0.6365 -0.0450 0.051 Uiso 1 1 calc GR . . . .
C16 C 0.48093(18) 0.68814(14) 0.23109(14) 0.0305(4) Uani 1 1 d . . . . .
H16A H 0.5087 0.6882 0.2863 0.037 Uiso 1 1 calc R . . . .
H16B H 0.4081 0.6459 0.2556 0.037 Uiso 1 1 calc R . . . .
C17 C 0.42715(18) 0.79158(14) 0.18320(14) 0.0301(4) Uani 1 1 d . . . . .
C18 C 0.38254(18) 0.81191(15) 0.10179(14) 0.0318(4) Uani 1 1 d . . . . .
C19 C 0.34094(18) 0.90879(16) 0.05402(15) 0.0353(5) Uani 1 1 d . . . . .
C20 C 0.33739(19) 0.98360(16) 0.09209(16) 0.0384(5) Uani 1 1 d . . . . .
H20 H 0.3075 1.0494 0.0605 0.046 Uiso 1 1 calc R . . . .
C21 C 0.37583(19) 0.96609(15) 0.17453(16) 0.0373(5) Uani 1 1 d . . . . .
C22 C 0.42260(18) 0.86910(15) 0.21790(14) 0.0320(4) Uani 1 1 d . . . . .
H22 H 0.4524 0.8556 0.2731 0.038 Uiso 1 1 calc R . . . .
C23 C 0.3020(2) 0.93018(19) -0.03650(16) 0.0471(6) Uani 1 1 d . . . . .
H23A H 0.2225 0.8982 -0.0228 0.071 Uiso 1 1 calc GR . . . .
H23B H 0.3779 0.9048 -0.0836 0.071 Uiso 1 1 calc GR . . . .
H23C H 0.2802 1.0015 -0.0622 0.071 Uiso 1 1 calc GR . . . .
C24 C 0.3672(2) 1.04823(17) 0.21625(18) 0.0476(6) Uani 1 1 d . . . . .
H24A H 0.2831 1.0499 0.2683 0.071 Uiso 1 1 calc GR . . . .
H24B H 0.3675 1.1112 0.1663 0.071 Uiso 1 1 calc GR . . . .
H24C H 0.4452 1.0369 0.2412 0.071 Uiso 1 1 calc GR . . . .
O3' O 0.05889(15) 0.12689(10) 0.36976(10) 0.0393(4) Uani 1 1 d . . . . .
N1' N -0.08962(15) 0.22598(11) 0.50274(11) 0.0263(3) Uani 1 1 d . . . . .
O1' O 0.09002(12) 0.36403(9) 0.40315(9) 0.0300(3) Uani 1 1 d . . . . .
H1' H 0.0674 0.3075 0.4321 0.045 Uiso 1 1 calc GR . . . .
C2' C -0.1519(2) 0.22524(14) 0.43088(14) 0.0314(4) Uani 1 1 d . . . . .
H2' H -0.1680 0.2953 0.3925 0.038 Uiso 1 1 calc R . . . .
O2' O 0.20646(14) 0.08729(11) 0.49775(10) 0.0366(3) Uani 1 1 d . . . . .
H2'A H 0.1451 0.1061 0.4698 0.055 Uiso 1 1 calc GR . . . .
C3' C -0.2895(2) 0.18635(17) 0.47004(17) 0.0416(5) Uani 1 1 d . . . . .
H3'A H -0.2766 0.1154 0.5011 0.062 Uiso 1 1 calc GR . . . .
H3'B H -0.3288 0.1988 0.4172 0.062 Uiso 1 1 calc GR . . . .
H3'C H -0.3510 0.2201 0.5168 0.062 Uiso 1 1 calc GR . . . .
O4' O -0.09981(16) 0.17674(10) 0.29100(10) 0.0415(4) Uani 1 1 d . . . . .
C4' C -0.0516(2) 0.17059(14) 0.36217(14) 0.0326(4) Uani 1 1 d . . . . .
C5' C -0.0114(3) 0.12759(16) 0.21928(16) 0.0527(7) Uani 1 1 d . . . . .
H5'A H 0.0207 0.0587 0.2508 0.063 Uiso 1 1 calc R . . . .
H5'B H 0.0686 0.1623 0.1814 0.063 Uiso 1 1 calc R . . . .
C6' C -0.0935(4) 0.12988(19) 0.15566(19) 0.0702(9) Uani 1 1 d . . . . .
H6'A H -0.1239 0.1984 0.1245 0.105 Uiso 1 1 calc GR . . . .
H6'B H -0.1727 0.0958 0.1941 0.105 Uiso 1 1 calc GR . . . .
H6'C H -0.0377 0.0970 0.1068 0.105 Uiso 1 1 calc GR . . . .
C7' C -0.15820(19) 0.30529(13) 0.54859(13) 0.0288(4) Uani 1 1 d . . . . .
H7'A H -0.1208 0.2965 0.6022 0.035 Uiso 1 1 calc R . . . .
H7'B H -0.2559 0.2983 0.5762 0.035 Uiso 1 1 calc R . . . .
C8' C -0.14487(18) 0.40806(13) 0.48319(13) 0.0259(4) Uani 1 1 d . . . . .
C9' C -0.02153(18) 0.43341(13) 0.41788(13) 0.0257(4) Uani 1 1 d . . . . .
C10' C -0.00634(19) 0.53189(14) 0.36605(13) 0.0278(4) Uani 1 1 d . . . . .
C11' C -0.1179(2) 0.60333(14) 0.38243(14) 0.0308(4) Uani 1 1 d . . . . .
H11' H -0.1085 0.6703 0.3483 0.037 Uiso 1 1 calc R . . . .
C12' C -0.2424(2) 0.58051(14) 0.44672(14) 0.0313(4) Uani 1 1 d . . . . .
C13' C -0.25405(19) 0.48216(14) 0.49567(13) 0.0296(4) Uani 1 1 d . . . . .
H13' H -0.3389 0.4649 0.5389 0.036 Uiso 1 1 calc R . . . .
C14' C 0.1276(2) 0.55783(15) 0.29752(14) 0.0337(4) Uani 1 1 d . . . . .
H14D H 0.1511 0.5263 0.2462 0.051 Uiso 1 1 calc GR . . . .
H14E H 0.1977 0.5347 0.3315 0.051 Uiso 1 1 calc GR . . . .
H14F H 0.1216 0.6294 0.2700 0.051 Uiso 1 1 calc GR . . . .
C15' C -0.3607(2) 0.65974(16) 0.46479(17) 0.0440(5) Uani 1 1 d . . . . .
H15D H -0.4448 0.6300 0.4961 0.066 Uiso 1 1 calc GR . . . .
H15E H -0.3668 0.7080 0.4038 0.066 Uiso 1 1 calc GR . . . .
H15F H -0.3472 0.6927 0.5063 0.066 Uiso 1 1 calc GR . . . .
C16' C -0.08528(19) 0.13053(13) 0.57836(13) 0.0281(4) Uani 1 1 d . . . . .
H16C H -0.0611 0.0757 0.5490 0.034 Uiso 1 1 calc R . . . .
H16D H -0.1762 0.1247 0.6249 0.034 Uiso 1 1 calc R . . . .
C17' C 0.01728(18) 0.12310(13) 0.62979(13) 0.0264(4) Uani 1 1 d . . . . .
C18' C 0.15627(19) 0.10225(13) 0.58690(13) 0.0288(4) Uani 1 1 d . . . . .
C19' C 0.25137(19) 0.09320(14) 0.63499(14) 0.0314(4) Uani 1 1 d . . . . .
C20' C 0.20596(19) 0.10811(13) 0.72512(14) 0.0312(4) Uani 1 1 d . . . . .
H20' H 0.2707 0.1040 0.7572 0.037 Uiso 1 1 calc R . . . .
C21' C 0.06778(19) 0.12906(13) 0.77037(13) 0.0292(4) Uani 1 1 d . . . . .
C22' C -0.02381(18) 0.13579(13) 0.72066(13) 0.0268(4) Uani 1 1 d . . . . .
H22' H -0.1181 0.1496 0.7501 0.032 Uiso 1 1 calc R . . . .
C23' C 0.3999(2) 0.06673(17) 0.58936(16) 0.0421(5) Uani 1 1 d . . . . .
H23D H 0.4171 -0.0018 0.5876 0.063 Uiso 1 1 calc GR . . . .
H23E H 0.4535 0.0747 0.6268 0.063 Uiso 1 1 calc GR . . . .
H23F H 0.4259 0.1101 0.5240 0.063 Uiso 1 1 calc GR . . . .
C24' C 0.0210(2) 0.14082(15) 0.87006(14) 0.0357(5) Uani 1 1 d . . . . .
H24D H 0.0028 0.0771 0.9169 0.054 Uiso 1 1 calc GR . . . .
H24E H -0.0622 0.1881 0.8768 0.054 Uiso 1 1 calc GR . . . .
H24F H 0.0919 0.1649 0.8812 0.054 Uiso 1 1 calc GR . . . .


_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
O3 C4 1.212(2) . ?
N1 C2 1.469(2) . ?
N1 C7 1.478(2) . ?
N1 C16 1.479(2) . ?
O1 H1 0.8400 . ?
O1 C9 1.378(2) . ?
C2 H2 1.0000 . ?
C2 C3 1.528(3) . ?
C2 C4 1.517(3) . ?
O2 H2A 0.8400 . ?
O2 C18 1.367(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
O4 C4 1.325(2) . ?
O4 C5 1.463(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.483(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.509(3) . ?
C8 C9 1.393(3) . ?
C8 C13 1.395(3) . ?
C9 C10 1.398(3) . ?
C10 C11 1.387(3) . ?
C10 C14 1.498(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.388(3) . ?
C12 C13 1.391(3) . ?
C12 C15 1.503(3) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.506(3) . ?
C17 C18 1.403(3) . ?
C17 C22 1.388(3) . ?
C18 C19 1.398(3) . ?
C19 C20 1.389(3) . ?
C19 C23 1.500(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.389(3) . ?
C21 C22 1.395(3) . ?
C21 C24 1.510(3) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O3' C4' 1.214(2) . ?
N1' C2' 1.471(2) . ?
N1' C7' 1.475(2) . ?
N1' C16' 1.487(2) . ?
O1' H1' 0.8400 . ?
O1' C9' 1.371(2) . ?
C2' H2' 1.0000 . ?
C2' C3' 1.536(3) . ?
C2' C4' 1.518(3) . ?
O2' H2'A 0.8400 . ?
O2' C18' 1.373(2) . ?
C3' H3'A 0.9800 . ?
C3' H3'B 0.9800 . ?
C3' H3'C 0.9800 . ?
O4' C4' 1.327(2) . ?
O4' C5' 1.463(3) . ?
C5' H5'A 0.9900 . ?
C5' H5'B 0.9900 . ?
C5' C6' 1.500(4) . ?
C6' H6'A 0.9800 . ?
C6' H6'B 0.9800 . ?
C6' H6'C 0.9800 . ?
C7' H7'A 0.9900 . ?
C7' H7'B 0.9900 . ?
C7' C8' 1.505(2) . ?
C8' C9' 1.394(3) . ?
C8' C13' 1.393(2) . ?
C9' C10' 1.404(3) . ?
C10' C11' 1.392(3) . ?
C10' C14' 1.496(3) . ?
C11' H11' 0.9500 . ?
C11' C12' 1.390(3) . ?
C12' C13' 1.388(3) . ?
C12' C15' 1.509(3) . ?
C13' H13' 0.9500 . ?
C14' H14D 0.9800 . ?
C14' H14E 0.9800 . ?
C14' H14F 0.9800 . ?
C15' H15D 0.9800 . ?
C15' H15E 0.9800 . ?
C15' H15F 0.9800 . ?
C16' H16C 0.9900 . ?
C16' H16D 0.9900 . ?
C16' C17' 1.508(3) . ?
C17' C18' 1.400(3) . ?
C17' C22' 1.387(3) . ?
C18' C19' 1.395(3) . ?
C19' C20' 1.387(3) . ?
C19' C23' 1.505(3) . ?
C20' H20' 0.9500 . ?
C20' C21' 1.401(3) . ?
C21' C22' 1.390(3) . ?
C21' C24' 1.508(3) . ?
C22' H22' 0.9500 . ?
C23' H23D 0.9800 . ?
C23' H23E 0.9800 . ?
C23' H23F 0.9800 . ?
C24' H24D 0.9800 . ?
C24' H24E 0.9800 . ?
C24' H24F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C7 111.89(14) . . ?
C2 N1 C16 113.55(14) . . ?
C7 N1 C16 110.79(15) . . ?
C9 O1 H1 109.5 . . ?
N1 C2 H2 105.8 . . ?
N1 C2 C3 116.70(17) . . ?
N1 C2 C4 109.20(15) . . ?
C3 C2 H2 105.8 . . ?
C4 C2 H2 105.8 . . ?
C4 C2 C3 112.80(17) . . ?
C18 O2 H2A 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 O4 C5 116.58(16) . . ?
O3 C4 C2 124.69(18) . . ?
O3 C4 O4 123.99(19) . . ?
O4 C4 C2 111.31(17) . . ?
O4 C5 H5A 110.3 . . ?
O4 C5 H5B 110.3 . . ?
O4 C5 C6 107.12(19) . . ?
H5A C5 H5B 108.5 . . ?
C6 C5 H5A 110.3 . . ?
C6 C5 H5B 110.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 109.1 . . ?
N1 C7 H7B 109.1 . . ?
N1 C7 C8 112.39(15) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
C9 C8 C7 120.76(16) . . ?
C9 C8 C13 118.45(17) . . ?
C13 C8 C7 120.77(17) . . ?
O1 C9 C8 122.10(16) . . ?
O1 C9 C10 116.60(17) . . ?
C8 C9 C10 121.30(17) . . ?
C9 C10 C14 120.58(17) . . ?
C11 C10 C9 117.63(17) . . ?
C11 C10 C14 121.80(17) . . ?
C10 C11 H11 118.4 . . ?
C10 C11 C12 123.29(18) . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C13 117.14(17) . . ?
C11 C12 C15 121.13(17) . . ?
C13 C12 C15 121.73(18) . . ?
C8 C13 H13 119.0 . . ?
C12 C13 C8 122.09(18) . . ?
C12 C13 H13 119.0 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 H16A 109.4 . . ?
N1 C16 H16B 109.4 . . ?
N1 C16 C17 111.21(15) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C18 C17 C16 120.82(18) . . ?
C22 C17 C16 120.61(18) . . ?
C22 C17 C18 118.57(18) . . ?
O2 C18 C17 123.19(18) . . ?
O2 C18 C19 116.24(18) . . ?
C19 C18 C17 120.57(19) . . ?
C18 C19 C23 120.1(2) . . ?
C20 C19 C18 118.5(2) . . ?
C20 C19 C23 121.5(2) . . ?
C19 C20 H20 118.7 . . ?
C21 C20 C19 122.62(19) . . ?
C21 C20 H20 118.7 . . ?
C20 C21 C22 117.3(2) . . ?
C20 C21 C24 121.7(2) . . ?
C22 C21 C24 121.0(2) . . ?
C17 C22 C21 122.3(2) . . ?
C17 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C2' N1' C7' 112.15(14) . . ?
C2' N1' C16' 113.10(15) . . ?
C7' N1' C16' 108.95(14) . . ?
C9' O1' H1' 109.5 . . ?
N1' C2' H2' 106.6 . . ?
N1' C2' C3' 116.08(16) . . ?
N1' C2' C4' 109.66(16) . . ?
C3' C2' H2' 106.6 . . ?
C4' C2' H2' 106.6 . . ?
C4' C2' C3' 110.87(17) . . ?
C18' O2' H2'A 109.5 . . ?
C2' C3' H3'A 109.5 . . ?
C2' C3' H3'B 109.5 . . ?
C2' C3' H3'C 109.5 . . ?
H3'A C3' H3'B 109.5 . . ?
H3'A C3' H3'C 109.5 . . ?
H3'B C3' H3'C 109.5 . . ?
C4' O4' C5' 116.30(18) . . ?
O3' C4' C2' 125.37(18) . . ?
O3' C4' O4' 123.45(18) . . ?
O4' C4' C2' 111.17(17) . . ?
O4' C5' H5'A 110.3 . . ?
O4' C5' H5'B 110.3 . . ?
O4' C5' C6' 107.1(2) . . ?
H5'A C5' H5'B 108.5 . . ?
C6' C5' H5'A 110.3 . . ?
C6' C5' H5'B 110.3 . . ?
C5' C6' H6'A 109.5 . . ?
C5' C6' H6'B 109.5 . . ?
C5' C6' H6'C 109.5 . . ?
H6'A C6' H6'B 109.5 . . ?
H6'A C6' H6'C 109.5 . . ?
H6'B C6' H6'C 109.5 . . ?
N1' C7' H7'A 108.5 . . ?
N1' C7' H7'B 108.5 . . ?
N1' C7' C8' 114.96(15) . . ?
H7'A C7' H7'B 107.5 . . ?
C8' C7' H7'A 108.5 . . ?
C8' C7' H7'B 108.5 . . ?
C9' C8' C7' 121.62(16) . . ?
C13' C8' C7' 119.09(16) . . ?
C13' C8' C9' 118.88(17) . . ?
O1' C9' C8' 121.65(16) . . ?
O1' C9' C10' 117.43(16) . . ?
C8' C9' C10' 120.91(16) . . ?
C9' C10' C14' 120.11(17) . . ?
C11' C10' C9' 117.95(17) . . ?
C11' C10' C14' 121.92(17) . . ?
C10' C11' H11' 118.7 . . ?
C12' C11' C10' 122.60(18) . . ?
C12' C11' H11' 118.7 . . ?
C11' C12' C15' 121.46(18) . . ?
C13' C12' C11' 117.77(17) . . ?
C13' C12' C15' 120.76(18) . . ?
C8' C13' H13' 119.1 . . ?
C12' C13' C8' 121.88(17) . . ?
C12' C13' H13' 119.1 . . ?
C10' C14' H14D 109.5 . . ?
C10' C14' H14E 109.5 . . ?
C10' C14' H14F 109.5 . . ?
H14D C14' H14E 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
C12' C15' H15D 109.5 . . ?
C12' C15' H15E 109.5 . . ?
C12' C15' H15F 109.5 . . ?
H15D C15' H15E 109.5 . . ?
H15D C15' H15F 109.5 . . ?
H15E C15' H15F 109.5 . . ?
N1' C16' H16C 109.5 . . ?
N1' C16' H16D 109.5 . . ?
N1' C16' C17' 110.83(15) . . ?
H16C C16' H16D 108.1 . . ?
C17' C16' H16C 109.5 . . ?
C17' C16' H16D 109.5 . . ?
C18' C17' C16' 120.51(17) . . ?
C22' C17' C16' 120.88(16) . . ?
C22' C17' C18' 118.60(18) . . ?
O2' C18' C17' 122.79(18) . . ?
O2' C18' C19' 116.45(16) . . ?
C19' C18' C17' 120.74(18) . . ?
C18' C19' C23' 119.97(18) . . ?
C20' C19' C18' 118.73(17) . . ?
C20' C19' C23' 121.30(19) . . ?
C19' C20' H20' 118.9 . . ?
C19' C20' C21' 122.17(19) . . ?
C21' C20' H20' 118.9 . . ?
C20' C21' C24' 121.03(18) . . ?
C22' C21' C20' 117.27(18) . . ?
C22' C21' C24' 121.68(17) . . ?
C17' C22' C21' 122.47(17) . . ?
C17' C22' H22' 118.8 . . ?
C21' C22' H22' 118.8 . . ?
C19' C23' H23D 109.5 . . ?
C19' C23' H23E 109.5 . . ?
C19' C23' H23F 109.5 . . ?
H23D C23' H23E 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
C21' C24' H24D 109.5 . . ?
C21' C24' H24E 109.5 . . ?
C21' C24' H24F 109.5 . . ?
H24D C24' H24E 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C4 O3 11.1(3) . . . . ?
N1 C2 C4 O4 -170.03(15) . . . . ?
N1 C7 C8 C9 48.2(2) . . . . ?
N1 C7 C8 C13 -133.49(18) . . . . ?
N1 C16 C17 C18 58.2(2) . . . . ?
N1 C16 C17 C22 -120.87(19) . . . . ?
O1 C9 C10 C11 177.36(16) . . . . ?
O1 C9 C10 C14 -2.4(3) . . . . ?
C2 N1 C7 C8 59.6(2) . . . . ?
C2 N1 C16 C17 -162.14(16) . . . . ?
O2 C18 C19 C20 176.96(17) . . . . ?
O2 C18 C19 C23 -3.3(3) . . . . ?
C3 C2 C4 O3 142.6(2) . . . . ?
C3 C2 C4 O4 -38.5(2) . . . . ?
C4 O4 C5 C6 -177.1(2) . . . . ?
C5 O4 C4 O3 -0.9(3) . . . . ?
C5 O4 C4 C2 -179.77(18) . . . . ?
C7 N1 C2 C3 68.3(2) . . . . ?
C7 N1 C2 C4 -162.35(15) . . . . ?
C7 N1 C16 C17 71.0(2) . . . . ?
C7 C8 C9 O1 -1.6(3) . . . . ?
C7 C8 C9 C10 177.81(16) . . . . ?
C7 C8 C13 C12 -175.29(17) . . . . ?
C8 C9 C10 C11 -2.1(3) . . . . ?
C8 C9 C10 C14 178.14(17) . . . . ?
C9 C8 C13 C12 3.1(3) . . . . ?
C9 C10 C11 C12 2.4(3) . . . . ?
C10 C11 C12 C13 -0.1(3) . . . . ?
C10 C11 C12 C15 -179.54(17) . . . . ?
C11 C12 C13 C8 -2.7(3) . . . . ?
C13 C8 C9 O1 -179.98(16) . . . . ?
C13 C8 C9 C10 -0.6(3) . . . . ?
C14 C10 C11 C12 -177.78(18) . . . . ?
C15 C12 C13 C8 176.70(17) . . . . ?
C16 N1 C2 C3 -58.1(2) . . . . ?
C16 N1 C2 C4 71.3(2) . . . . ?
C16 N1 C7 C8 -172.57(15) . . . . ?
C16 C17 C18 O2 3.5(3) . . . . ?
C16 C17 C18 C19 -175.86(16) . . . . ?
C16 C17 C22 C21 178.81(17) . . . . ?
C17 C18 C19 C20 -3.7(3) . . . . ?
C17 C18 C19 C23 176.05(17) . . . . ?
C18 C17 C22 C21 -0.2(3) . . . . ?
C18 C19 C20 C21 1.2(3) . . . . ?
C19 C20 C21 C22 1.6(3) . . . . ?
C19 C20 C21 C24 -178.15(19) . . . . ?
C20 C21 C22 C17 -2.1(3) . . . . ?
C22 C17 C18 O2 -177.48(17) . . . . ?
C22 C17 C18 C19 3.2(3) . . . . ?
C23 C19 C20 C21 -178.49(18) . . . . ?
C24 C21 C22 C17 177.65(18) . . . . ?
N1' C2' C4' O3' 5.8(3) . . . . ?
N1' C2' C4' O4' -173.94(15) . . . . ?
N1' C7' C8' C9' -43.6(3) . . . . ?
N1' C7' C8' C13' 143.87(18) . . . . ?
N1' C16' C17' C18' -76.7(2) . . . . ?
N1' C16' C17' C22' 103.92(19) . . . . ?
O1' C9' C10' C11' -178.20(16) . . . . ?
O1' C9' C10' C14' 0.3(3) . . . . ?
C2' N1' C7' C8' -66.2(2) . . . . ?
C2' N1' C16' C17' 161.30(15) . . . . ?
O2' C18' C19' C20' 179.67(16) . . . . ?
O2' C18' C19' C23' -0.9(3) . . . . ?
C3' C2' C4' O3' -123.7(2) . . . . ?
C3' C2' C4' O4' 56.6(2) . . . . ?
C4' O4' C5' C6' 171.09(18) . . . . ?
C5' O4' C4' O3' -0.3(3) . . . . ?
C5' O4' C4' C2' 179.40(16) . . . . ?
C7' N1' C2' C3' -74.1(2) . . . . ?
C7' N1' C2' C4' 159.34(15) . . . . ?
C7' N1' C16' C17' -73.25(18) . . . . ?
C7' C8' C9' O1' 6.7(3) . . . . ?
C7' C8' C9' C10' -171.86(17) . . . . ?
C7' C8' C13' C12' 171.14(18) . . . . ?
C8' C9' C10' C11' 0.4(3) . . . . ?
C8' C9' C10' C14' 178.93(18) . . . . ?
C9' C8' C13' C12' -1.6(3) . . . . ?
C9' C10' C11' C12' -0.7(3) . . . . ?
C10' C11' C12' C13' -0.1(3) . . . . ?
C10' C11' C12' C15' 178.52(19) . . . . ?
C11' C12' C13' C8' 1.3(3) . . . . ?
C13' C8' C9' O1' 179.29(17) . . . . ?
C13' C8' C9' C10' 0.7(3) . . . . ?
C14' C10' C11' C12' -179.20(19) . . . . ?
C15' C12' C13' C8' -177.32(19) . . . . ?
C16' N1' C2' C3' 49.6(2) . . . . ?
C16' N1' C2' C4' -76.95(18) . . . . ?
C16' N1' C7' C8' 167.84(16) . . . . ?
C16' C17' C18' O2' -0.2(3) . . . . ?
C16' C17' C18' C19' -178.61(17) . . . . ?
C16' C17' C22' C21' 179.72(16) . . . . ?
C17' C18' C19' C20' -1.9(3) . . . . ?
C17' C18' C19' C23' 177.53(18) . . . . ?
C18' C17' C22' C21' 0.3(3) . . . . ?
C18' C19' C20' C21' 1.9(3) . . . . ?
C19' C20' C21' C22' -0.8(3) . . . . ?
C19' C20' C21' C24' 177.47(18) . . . . ?
C20' C21' C22' C17' -0.3(3) . . . . ?
C22' C17' C18' O2' 179.16(16) . . . . ?
C22' C17' C18' C19' 0.8(3) . . . . ?
C23' C19' C20' C21' -177.49(18) . . . . ?
C24' C21' C22' C17' -178.59(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_dj56
_database_code_depnum_ccdc_archive 'CCDC 2070853'
loop_
_audit_author_name
_audit_author_address
'Georgina Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-11-03 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT244_dj56                
;
PROBLEM: Low    'Solvent' Ueq as Compared to Neighbors of        C30 Check
RESPONSE: There are small residual peaks near Cl of 0.37 e\%A , attempts to model ;these as an extra conformation of the solvent did not result in a stable refinement ,with  large Ueq values for the Cl atoms . 0.37 is only 2% f the electron count of a Cl atom so an alternative orientation was not modelled 
;
# Added during the CSD deposition process: Wednesday 03 November 2021 03:33 PM
# end Validation Reply Form

_audit_creation_date             2021-11-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H2 Cl2, C29 H35 N O4'
_chemical_formula_sum            'C30 H37 Cl2 N O4'
_chemical_formula_weight         546.50
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.3845(4)
_cell_length_b                   16.8171(4)
_cell_length_c                   11.7263(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.9650(10)
_cell_angle_gamma                90
_cell_volume                     2793.86(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      62.547
_cell_measurement_theta_min      4.080
_shelx_estimated_absorpt_T_max   0.911
_shelx_estimated_absorpt_T_min   0.517
_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.5266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1307 before and 0.0885 after correction.
The Ratio of minimum to maximum transmission is 0.7001.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33650
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.601
_diffrn_reflns_theta_min         3.119
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4477
_reflns_number_total             5696
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5696
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0631
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)²+4.2436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1719
_refine_special_details          ?
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C16(H16A,H16B), C20(H20A,H20B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C22(H22), C26(H26),
 C29(H29)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C28(H28A,H28B,H28C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.30383(6) 0.56069(5) 0.79670(7) 0.0437(2) Uani 1 1 d . . . . .
Cl2 Cl 0.19510(7) 0.59867(7) 0.97797(9) 0.0601(3) Uani 1 1 d . . . . .
O4 O 0.22374(14) 0.51051(10) 0.49542(16) 0.0256(4) Uani 1 1 d . . . . .
O3 O 0.12918(14) 0.45185(11) 0.60276(17) 0.0273(4) Uani 1 1 d . . . . .
O1 O 0.27411(13) 0.35315(11) 0.84324(16) 0.0250(4) Uani 1 1 d . . . . .
H1 H 0.238255 0.345362 0.779679 0.038 Uiso 1 1 calc R U . . .
O2 O 0.03791(14) 0.33966(11) 0.71251(17) 0.0284(4) Uani 1 1 d . . . . .
H2 H 0.070282 0.361198 0.667918 0.043 Uiso 1 1 calc R U . . .
N1 N 0.22782(15) 0.31200(12) 0.61436(18) 0.0191(4) Uani 1 1 d . . . . .
C1 C 0.6512(2) 0.2651(2) 0.8140(3) 0.0389(7) Uani 1 1 d . . . . .
H1A H 0.663205 0.211169 0.844537 0.058 Uiso 1 1 calc R U . . .
H1B H 0.695427 0.302197 0.859569 0.058 Uiso 1 1 calc R U . . .
H1C H 0.659988 0.266570 0.732961 0.058 Uiso 1 1 calc R U . . .
C2 C 0.5511(2) 0.28905(16) 0.8215(3) 0.0274(6) Uani 1 1 d . . . . .
C3 C 0.47688(19) 0.26684(15) 0.7355(2) 0.0245(6) Uani 1 1 d . . . . .
H3 H 0.490013 0.237345 0.671054 0.029 Uiso 1 1 calc R U . . .
C4 C 0.38331(19) 0.28660(15) 0.7409(2) 0.0207(5) Uani 1 1 d . . . . .
C5 C 0.30439(19) 0.25391(14) 0.6522(2) 0.0214(5) Uani 1 1 d . . . . .
H5A H 0.330559 0.236145 0.583745 0.026 Uiso 1 1 calc R U . . .
H5B H 0.277385 0.206761 0.685103 0.026 Uiso 1 1 calc R U . . .
C6 C 0.26092(18) 0.37797(14) 0.5492(2) 0.0193(5) Uani 1 1 d . . . . .
H6 H 0.324671 0.393517 0.591768 0.023 Uiso 1 1 calc R U . . .
C7 C 0.27312(19) 0.35693(15) 0.4233(2) 0.0212(5) Uani 1 1 d . . . . .
H7A H 0.290051 0.300002 0.420264 0.025 Uiso 1 1 calc R U . . .
H7B H 0.211938 0.364717 0.371062 0.025 Uiso 1 1 calc R U . . .
C8 C 0.34764(19) 0.40606(15) 0.3791(2) 0.0222(5) Uani 1 1 d . . . . .
C9 C 0.3223(2) 0.46350(16) 0.2945(2) 0.0250(6) Uani 1 1 d . . . . .
H9 H 0.257521 0.470819 0.262457 0.030 Uiso 1 1 calc R U . . .
C10 C 0.3897(2) 0.51028(17) 0.2561(3) 0.0302(6) Uani 1 1 d . . . . .
H10 H 0.371052 0.549670 0.198581 0.036 Uiso 1 1 calc R U . . .
C11 C 0.4843(2) 0.49966(17) 0.3014(3) 0.0322(7) Uani 1 1 d . . . . .
H11 H 0.530746 0.532108 0.275904 0.039 Uiso 1 1 calc R U . . .
C12 C -0.0604(2) 0.25587(18) 0.8558(2) 0.0284(6) Uani 1 1 d . . . . .
H12A H -0.122376 0.270898 0.812463 0.043 Uiso 1 1 calc R U . . .
H12B H -0.026568 0.303688 0.887709 0.043 Uiso 1 1 calc R U . . .
H12C H -0.068576 0.219933 0.919056 0.043 Uiso 1 1 calc R U . . .
C13 C -0.00439(19) 0.21449(16) 0.7759(2) 0.0231(6) Uani 1 1 d . . . . .
C14 C 0.04413(18) 0.25889(15) 0.7041(2) 0.0214(5) Uani 1 1 d . . . . .
C15 C 0.09411(18) 0.22145(15) 0.6268(2) 0.0198(5) Uani 1 1 d . . . . .
C16 C 0.14466(19) 0.27062(15) 0.5481(2) 0.0209(5) Uani 1 1 d . . . . .
H16A H 0.165375 0.235519 0.489548 0.025 Uiso 1 1 calc R U . . .
H16B H 0.100429 0.310393 0.506853 0.025 Uiso 1 1 calc R U . . .
C17 C 0.5109(2) 0.44163(19) 0.3840(3) 0.0330(7) Uani 1 1 d . . . . .
H17 H 0.575818 0.433733 0.414707 0.040 Uiso 1 1 calc R U . . .
C18 C 0.4426(2) 0.39453(17) 0.4226(3) 0.0277(6) Uani 1 1 d . . . . .
H18 H 0.461254 0.354406 0.478929 0.033 Uiso 1 1 calc R U . . .
C19 C 0.19647(19) 0.44935(14) 0.5533(2) 0.0202(5) Uani 1 1 d . . . . .
C20 C 0.1690(2) 0.58363(15) 0.4940(2) 0.0277(6) Uani 1 1 d . . . . .
H20A H 0.173953 0.605240 0.573398 0.033 Uiso 1 1 calc R U . . .
H20B H 0.101654 0.573313 0.462785 0.033 Uiso 1 1 calc R U . . .
C21 C 0.2094(2) 0.64132(17) 0.4181(3) 0.0336(7) Uani 1 1 d . . . . .
H21A H 0.276460 0.649806 0.448851 0.050 Uiso 1 1 calc R U . . .
H21B H 0.175653 0.692046 0.416424 0.050 Uiso 1 1 calc R U . . .
H21C H 0.202486 0.619804 0.339415 0.050 Uiso 1 1 calc R U . . .
C22 C 0.5298(2) 0.33421(16) 0.9133(2) 0.0262(6) Uani 1 1 d . . . . .
H22 H 0.579738 0.349303 0.973453 0.031 Uiso 1 1 calc R U . . .
C23 C 0.4382(2) 0.35811(16) 0.9203(2) 0.0249(6) Uani 1 1 d . . . . .
C24 C 0.4190(2) 0.41189(17) 1.0163(2) 0.0297(6) Uani 1 1 d . . . . .
H24A H 0.411928 0.466754 0.987975 0.045 Uiso 1 1 calc R U . . .
H24B H 0.471773 0.408908 1.081394 0.045 Uiso 1 1 calc R U . . .
H24C H 0.360786 0.395016 1.042099 0.045 Uiso 1 1 calc R U . . .
C25 C 0.36518(19) 0.33240(15) 0.8335(2) 0.0220(5) Uani 1 1 d . . . . .
C26 C 0.09428(19) 0.13890(16) 0.6220(2) 0.0233(6) Uani 1 1 d . . . . .
H26 H 0.127164 0.113357 0.568596 0.028 Uiso 1 1 calc R U . . .
C27 C 0.04787(19) 0.09235(16) 0.6927(2) 0.0243(6) Uani 1 1 d . . . . .
C28 C 0.0471(2) 0.00259(17) 0.6839(3) 0.0339(7) Uani 1 1 d . . . . .
H28A H 0.036812 -0.020361 0.757529 0.051 Uiso 1 1 calc R U . . .
H28B H 0.107726 -0.015845 0.666550 0.051 Uiso 1 1 calc R U . . .
H28C H -0.003873 -0.014152 0.621890 0.051 Uiso 1 1 calc R U . . .
C29 C 0.00042(19) 0.13176(16) 0.7699(2) 0.0244(6) Uani 1 1 d . . . . .
H29 H -0.029939 0.101026 0.820734 0.029 Uiso 1 1 calc R U . . .
C30 C 0.2108(2) 0.53171(19) 0.8677(3) 0.0360(7) Uani 1 1 d . . . . .
H30A H 0.151647 0.528450 0.810470 0.043 Uiso 1 1 calc R U . . .
H30B H 0.224308 0.478141 0.901559 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C30 1.762(3) . ?
Cl2 C30 1.759(3) . ?
O4 C19 1.329(3) . ?
O4 C20 1.459(3) . ?
O3 C19 1.212(3) . ?
O1 H1 0.8400 . ?
O1 C25 1.379(3) . ?
O2 H2 0.8400 . ?
O2 C14 1.366(3) . ?
N1 C5 1.482(3) . ?
N1 C6 1.472(3) . ?
N1 C16 1.482(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.513(4) . ?
C2 C3 1.387(4) . ?
C2 C22 1.394(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.398(4) . ?
C4 C5 1.505(4) . ?
C4 C25 1.393(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6 1.0000 . ?
C6 C7 1.557(3) . ?
C6 C19 1.523(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.514(3) . ?
C8 C9 1.387(4) . ?
C8 C18 1.386(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(5) . ?
C11 H11 0.9500 . ?
C11 C17 1.381(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 C13 1.507(4) . ?
C13 C14 1.399(3) . ?
C13 C29 1.395(4) . ?
C14 C15 1.400(3) . ?
C15 C16 1.515(3) . ?
C15 C26 1.389(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17 0.9500 . ?
C17 C18 1.397(4) . ?
C18 H18 0.9500 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.501(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.394(4) . ?
C23 C24 1.506(4) . ?
C23 C25 1.399(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.392(4) . ?
C27 C28 1.513(4) . ?
C27 C29 1.393(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?

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
C19 O4 C20 116.8(2) . . ?
C25 O1 H1 109.5 . . ?
C14 O2 H2 109.5 . . ?
C5 N1 C16 109.75(19) . . ?
C6 N1 C5 111.22(19) . . ?
C6 N1 C16 112.7(2) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 C22 117.7(3) . . ?
C22 C2 C1 121.9(3) . . ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 121.9(3) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 119.9(2) . . ?
C25 C4 C3 118.6(3) . . ?
C25 C4 C5 121.4(2) . . ?
N1 C5 C4 113.5(2) . . ?
N1 C5 H5A 108.9 . . ?
N1 C5 H5B 108.9 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N1 C6 H6 106.8 . . ?
N1 C6 C7 114.9(2) . . ?
N1 C6 C19 108.90(19) . . ?
C7 C6 H6 106.8 . . ?
C19 C6 H6 106.8 . . ?
C19 C6 C7 112.2(2) . . ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 C6 113.8(2) . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C9 C8 C7 120.7(2) . . ?
C18 C8 C7 120.6(2) . . ?
C18 C8 C9 118.8(2) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.1(3) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.2 . . ?
C17 C11 C10 119.7(3) . . ?
C17 C11 H11 120.2 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
C14 C13 C12 120.2(2) . . ?
C29 C13 C12 121.9(2) . . ?
C29 C13 C14 117.9(2) . . ?
O2 C14 C13 116.2(2) . . ?
O2 C14 C15 122.8(2) . . ?
C13 C14 C15 121.0(2) . . ?
C14 C15 C16 120.2(2) . . ?
C26 C15 C14 118.7(2) . . ?
C26 C15 C16 121.1(2) . . ?
N1 C16 C15 111.5(2) . . ?
N1 C16 H16A 109.3 . . ?
N1 C16 H16B 109.3 . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C11 C17 H17 119.9 . . ?
C11 C17 C18 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C8 C18 C17 120.3(3) . . ?
C8 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
O4 C19 C6 111.0(2) . . ?
O3 C19 O4 123.3(2) . . ?
O3 C19 C6 125.7(2) . . ?
O4 C20 H20A 110.4 . . ?
O4 C20 H20B 110.4 . . ?
O4 C20 C21 106.7(2) . . ?
H20A C20 H20B 108.6 . . ?
C21 C20 H20A 110.4 . . ?
C21 C20 H20B 110.4 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C2 C22 H22 118.7 . . ?
C23 C22 C2 122.6(3) . . ?
C23 C22 H22 118.7 . . ?
C22 C23 C24 121.0(3) . . ?
C22 C23 C25 117.8(3) . . ?
C25 C23 C24 121.2(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 C25 C4 120.9(2) . . ?
O1 C25 C23 117.8(2) . . ?
C4 C25 C23 121.4(2) . . ?
C15 C26 H26 118.9 . . ?
C15 C26 C27 122.2(2) . . ?
C27 C26 H26 118.9 . . ?
C26 C27 C28 121.3(3) . . ?
C26 C27 C29 117.4(2) . . ?
C29 C27 C28 121.4(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C13 C29 H29 118.6 . . ?
C27 C29 C13 122.8(2) . . ?
C27 C29 H29 118.6 . . ?
Cl1 C30 H30A 109.2 . . ?
Cl1 C30 H30B 109.2 . . ?
Cl2 C30 Cl1 112.02(18) . . ?
Cl2 C30 H30A 109.2 . . ?
Cl2 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C14 C15 C16 0.2(4) . . . . ?
O2 C14 C15 C26 -178.2(2) . . . . ?
N1 C6 C7 C8 -151.7(2) . . . . ?
N1 C6 C19 O4 -180.0(2) . . . . ?
N1 C6 C19 O3 0.4(4) . . . . ?
C1 C2 C3 C4 178.7(3) . . . . ?
C1 C2 C22 C23 178.6(3) . . . . ?
C2 C3 C4 C5 -173.5(2) . . . . ?
C2 C3 C4 C25 2.4(4) . . . . ?
C2 C22 C23 C24 -175.5(2) . . . . ?
C2 C22 C23 C25 2.7(4) . . . . ?
C3 C2 C22 C23 -0.8(4) . . . . ?
C3 C4 C5 N1 -140.8(2) . . . . ?
C3 C4 C25 O1 -179.6(2) . . . . ?
C3 C4 C25 C23 -0.4(4) . . . . ?
C5 N1 C6 C7 75.1(3) . . . . ?
C5 N1 C6 C19 -158.1(2) . . . . ?
C5 N1 C16 C15 73.0(2) . . . . ?
C5 C4 C25 O1 -3.8(4) . . . . ?
C5 C4 C25 C23 175.5(2) . . . . ?
C6 N1 C5 C4 67.0(3) . . . . ?
C6 N1 C16 C15 -162.4(2) . . . . ?
C6 C7 C8 C9 -108.9(3) . . . . ?
C6 C7 C8 C18 71.0(3) . . . . ?
C7 C6 C19 O4 -51.6(3) . . . . ?
C7 C6 C19 O3 128.8(3) . . . . ?
C7 C8 C9 C10 178.1(2) . . . . ?
C7 C8 C18 C17 -178.1(2) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C9 C8 C18 C17 1.8(4) . . . . ?
C9 C10 C11 C17 0.7(4) . . . . ?
C10 C11 C17 C18 -0.8(4) . . . . ?
C11 C17 C18 C8 -0.5(4) . . . . ?
C12 C13 C14 O2 0.6(4) . . . . ?
C12 C13 C14 C15 -178.0(3) . . . . ?
C12 C13 C29 C27 176.7(3) . . . . ?
C13 C14 C15 C16 178.8(2) . . . . ?
C13 C14 C15 C26 0.4(4) . . . . ?
C14 C13 C29 C27 -2.7(4) . . . . ?
C14 C15 C16 N1 69.9(3) . . . . ?
C14 C15 C26 C27 -1.2(4) . . . . ?
C15 C26 C27 C28 178.5(3) . . . . ?
C15 C26 C27 C29 0.0(4) . . . . ?
C16 N1 C5 C4 -167.6(2) . . . . ?
C16 N1 C6 C7 -48.7(3) . . . . ?
C16 N1 C6 C19 78.2(2) . . . . ?
C16 C15 C26 C27 -179.6(2) . . . . ?
C18 C8 C9 C10 -1.8(4) . . . . ?
C19 O4 C20 C21 -176.6(2) . . . . ?
C19 C6 C7 C8 83.2(3) . . . . ?
C20 O4 C19 O3 0.7(4) . . . . ?
C20 O4 C19 C6 -178.9(2) . . . . ?
C22 C2 C3 C4 -1.8(4) . . . . ?
C22 C23 C25 O1 177.2(2) . . . . ?
C22 C23 C25 C4 -2.1(4) . . . . ?
C24 C23 C25 O1 -4.6(4) . . . . ?
C24 C23 C25 C4 176.1(2) . . . . ?
C25 C4 C5 N1 43.4(3) . . . . ?
C26 C15 C16 N1 -111.7(3) . . . . ?
C26 C27 C29 C13 2.0(4) . . . . ?
C28 C27 C29 C13 -176.5(3) . . . . ?
C29 C13 C14 O2 -179.9(2) . . . . ?
C29 C13 C14 C15 1.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
####################################################################### 
# 
# 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_ef125
_database_code_depnum_ccdc_archive 'CCDC 2060206'
loop_
_audit_author_name
_audit_author_address
'Georgina M. Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2020-11-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H62 N2 O4 Pd'
_chemical_formula_sum            'C46 H62 N2 O4 Pd'
_chemical_formula_weight         813.37
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   13.3749(3)
_cell_length_b                   10.4918(2)
_cell_length_c                   16.3394(3)
_cell_angle_alpha                90
_cell_angle_beta                 112.5780(10)
_cell_angle_gamma                90
_cell_volume                     2117.13(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2343
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      50.88
_cell_measurement_theta_min      3.66
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.698
_exptl_absorpt_coefficient_mu    3.867
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1467 before and 0.0840 after correction.
The Ratio of minimum to maximum transmission is 0.5488.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56149
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.889
_diffrn_reflns_theta_min         5.430
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                8317
_reflns_number_total             8347
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.026(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8347
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0179
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0139P)²+0.5721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0444
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.974(4)
 0.026(4)
2. 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
3.a Ternary CH refined with riding coordinates:
 C23(H23)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C24(H24A,H24B), C32(H32A,H32B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.71294(2) 0.70765(2) 0.32078(2) 0.01019(5) Uani 1 1 d . . . . .
O1 O 0.78996(12) 0.79120(15) 0.43884(10) 0.0127(3) Uani 1 1 d . . . . .
N1 N 0.57640(14) 0.66646(17) 0.34548(11) 0.0105(3) Uani 1 1 d . . . . .
C1 C 0.77732(17) 0.7509(2) 0.51224(14) 0.0108(4) Uani 1 1 d . . . . .
O2 O 0.64901(12) 0.62606(15) 0.20037(10) 0.0153(3) Uani 1 1 d . . . . .
N2 N 0.84453(15) 0.75570(19) 0.29186(12) 0.0147(4) Uani 1 1 d . . . . .
C2 C 0.86598(17) 0.7478(2) 0.59563(14) 0.0116(4) Uani 1 1 d . . . . .
O3 O 0.48720(14) 0.45354(17) 0.46095(11) 0.0213(3) Uani 1 1 d . . . . .
C3 C 0.84608(14) 0.7031(3) 0.66881(12) 0.0123(3) Uani 1 1 d . . . . .
H3 H 0.905155 0.699302 0.724534 0.015 Uiso 1 1 calc R U . . .
O4 O 0.37676(13) 0.52738(16) 0.32773(11) 0.0166(3) Uani 1 1 d . . . . .
C4 C 0.74437(18) 0.6638(2) 0.66455(14) 0.0127(4) Uani 1 1 d . . . . .
C5 C 0.65829(17) 0.67374(19) 0.58278(14) 0.0126(4) Uani 1 1 d . . . . .
H5 H 0.587659 0.650099 0.577900 0.015 Uiso 1 1 calc R U . . .
C6 C 0.67362(15) 0.7175(3) 0.50843(12) 0.0112(4) Uani 1 1 d . . . . .
C7 C 0.57832(17) 0.74189(19) 0.42406(14) 0.0122(4) Uani 1 1 d . . . . .
H7A H 0.577015 0.833686 0.409647 0.015 Uiso 1 1 calc R U . . .
H7B H 0.511437 0.722926 0.434136 0.015 Uiso 1 1 calc R U . . .
C8 C 0.48777(15) 0.7218(3) 0.26497(13) 0.0123(4) Uani 1 1 d . . . . .
H8A H 0.421015 0.727865 0.277304 0.015 Uiso 1 1 calc R U . . .
H8B H 0.508735 0.809553 0.255917 0.015 Uiso 1 1 calc R U . . .
C9 C 0.46217(18) 0.6488(2) 0.18046(14) 0.0125(4) Uani 1 1 d . . . . .
C10 C 0.54351(18) 0.6092(2) 0.15121(14) 0.0128(4) Uani 1 1 d . . . . .
C11 C 0.5112(2) 0.5500(2) 0.06646(15) 0.0151(4) Uani 1 1 d . . . . .
C12 C 0.4008(2) 0.5330(2) 0.01753(15) 0.0180(5) Uani 1 1 d . . . . .
H12 H 0.379619 0.491940 -0.038405 0.022 Uiso 1 1 calc R U . . .
C13 C 0.31916(19) 0.5727(2) 0.04562(15) 0.0170(4) Uani 1 1 d . . . . .
C14 C 0.35319(18) 0.6299(2) 0.12828(15) 0.0151(4) Uani 1 1 d . . . . .
H14 H 0.300307 0.657306 0.150063 0.018 Uiso 1 1 calc R U . . .
C15 C 0.1989(2) 0.5490(2) -0.01102(16) 0.0204(5) Uani 1 1 d . . . . .
C16 C 0.1684(2) 0.4150(3) 0.0072(2) 0.0325(6) Uani 1 1 d . . . . .
H16A H 0.213781 0.352553 -0.007036 0.049 Uiso 1 1 calc R U . . .
H16B H 0.092098 0.398886 -0.029500 0.049 Uiso 1 1 calc R U . . .
H16C H 0.179775 0.407462 0.069965 0.049 Uiso 1 1 calc R U . . .
C17 C 0.1267(2) 0.6458(3) 0.0104(2) 0.0387(7) Uani 1 1 d . . . . .
H17A H 0.133449 0.634181 0.071846 0.058 Uiso 1 1 calc R U . . .
H17B H 0.051113 0.632659 -0.029655 0.058 Uiso 1 1 calc R U . . .
H17C H 0.149162 0.732355 0.002772 0.058 Uiso 1 1 calc R U . . .
C18 C 0.1764(2) 0.5622(4) -0.10995(18) 0.0382(8) Uani 1 1 d . . . . .
H18A H 0.204205 0.644222 -0.120678 0.057 Uiso 1 1 calc R U . . .
H18B H 0.098152 0.557906 -0.144233 0.057 Uiso 1 1 calc R U . . .
H18C H 0.212355 0.492806 -0.128206 0.057 Uiso 1 1 calc R U . . .
C19 C 0.5947(2) 0.5114(2) 0.02745(15) 0.0188(5) Uani 1 1 d . . . . .
C20 C 0.6759(2) 0.4136(3) 0.08712(17) 0.0228(5) Uani 1 1 d . . . . .
H20A H 0.710758 0.448529 0.147082 0.034 Uiso 1 1 calc R U . . .
H20B H 0.731066 0.395243 0.062985 0.034 Uiso 1 1 calc R U . . .
H20C H 0.637593 0.334899 0.089287 0.034 Uiso 1 1 calc R U . . .
C21 C 0.5426(2) 0.4484(3) -0.06455(17) 0.0263(6) Uani 1 1 d . . . . .
H21A H 0.501275 0.373259 -0.060390 0.039 Uiso 1 1 calc R U . . .
H21B H 0.599396 0.422555 -0.085148 0.039 Uiso 1 1 calc R U . . .
H21C H 0.493961 0.509341 -0.106586 0.039 Uiso 1 1 calc R U . . .
C22 C 0.6535(2) 0.6324(2) 0.01595(16) 0.0225(5) Uani 1 1 d . . . . .
H22A H 0.602011 0.687543 -0.029023 0.034 Uiso 1 1 calc R U . . .
H22B H 0.712153 0.608284 -0.002913 0.034 Uiso 1 1 calc R U . . .
H22C H 0.683627 0.678177 0.072465 0.034 Uiso 1 1 calc R U . . .
C23 C 0.56303(17) 0.5252(2) 0.35502(14) 0.0118(4) Uani 1 1 d . . . . .
H23 H 0.538634 0.488034 0.294093 0.014 Uiso 1 1 calc R U . . .
C24 C 0.66799(18) 0.4558(2) 0.41144(15) 0.0149(4) Uani 1 1 d . . . . .
H24A H 0.730554 0.499916 0.405975 0.018 Uiso 1 1 calc R U . . .
H24B H 0.677257 0.458103 0.474520 0.018 Uiso 1 1 calc R U . . .
C25 C 0.6653(2) 0.3189(2) 0.38196(18) 0.0145(5) Uani 1 1 d . . . . .
C26 C 0.6581(2) 0.2920(3) 0.29665(17) 0.0168(5) Uani 1 1 d . . . . .
H26 H 0.651979 0.359863 0.256498 0.020 Uiso 1 1 calc R U . . .
C27 C 0.6597(2) 0.1671(2) 0.26951(18) 0.0209(5) Uani 1 1 d . . . . .
H27 H 0.655497 0.149888 0.211179 0.025 Uiso 1 1 calc R U . . .
C28 C 0.6676(2) 0.0670(2) 0.32724(19) 0.0233(5) Uani 1 1 d . . . . .
H28 H 0.668769 -0.018617 0.308677 0.028 Uiso 1 1 calc R U . . .
C29 C 0.6737(3) 0.0929(3) 0.4116(2) 0.0257(6) Uani 1 1 d . . . . .
H29 H 0.679224 0.024661 0.451367 0.031 Uiso 1 1 calc R U . . .
C30 C 0.67170(18) 0.2176(3) 0.43909(14) 0.0214(5) Uani 1 1 d . . . . .
H30 H 0.674753 0.234142 0.497163 0.026 Uiso 1 1 calc R U . . .
C31 C 0.47370(18) 0.4966(2) 0.38943(15) 0.0139(4) Uani 1 1 d . . . . .
C32 C 0.28262(19) 0.5058(2) 0.35023(16) 0.0180(5) Uani 1 1 d . . . . .
H32A H 0.279614 0.570076 0.393575 0.022 Uiso 1 1 calc R U . . .
H32B H 0.285778 0.419888 0.376202 0.022 Uiso 1 1 calc R U . . .
C33 C 0.1851(2) 0.5174(3) 0.26462(19) 0.0292(6) Uani 1 1 d . . . . .
H33A H 0.190815 0.455505 0.221685 0.044 Uiso 1 1 calc R U . . .
H33B H 0.181799 0.603748 0.240884 0.044 Uiso 1 1 calc R U . . .
H33C H 0.119280 0.500407 0.275611 0.044 Uiso 1 1 calc R U . . .
C34 C 0.72320(18) 0.6152(2) 0.74523(14) 0.0150(4) Uani 1 1 d . . . . .
C35 C 0.6773(2) 0.4793(2) 0.72652(16) 0.0229(5) Uani 1 1 d . . . . .
H35A H 0.608363 0.480257 0.675186 0.034 Uiso 1 1 calc R U . . .
H35B H 0.665605 0.446957 0.778403 0.034 Uiso 1 1 calc R U . . .
H35C H 0.728765 0.423886 0.714024 0.034 Uiso 1 1 calc R U . . .
C36 C 0.63993(16) 0.7020(4) 0.76176(13) 0.0213(4) Uani 1 1 d . . . . .
H36A H 0.667540 0.789518 0.771983 0.032 Uiso 1 1 calc R U . . .
H36B H 0.627768 0.671677 0.813923 0.032 Uiso 1 1 calc R U . . .
H36C H 0.571523 0.699948 0.709897 0.032 Uiso 1 1 calc R U . . .
C37 C 0.82627(19) 0.6125(3) 0.82989(15) 0.0194(5) Uani 1 1 d . . . . .
H37A H 0.879431 0.555331 0.821364 0.029 Uiso 1 1 calc R U . . .
H37B H 0.808672 0.581717 0.879410 0.029 Uiso 1 1 calc R U . . .
H37C H 0.856587 0.698605 0.843010 0.029 Uiso 1 1 calc R U . . .
C38 C 0.97895(17) 0.7949(2) 0.60555(14) 0.0140(4) Uani 1 1 d . . . . .
C39 C 1.02277(15) 0.7110(4) 0.54963(13) 0.0189(4) Uani 1 1 d . . . . .
H39A H 0.971883 0.712467 0.487628 0.028 Uiso 1 1 calc R U . . .
H39B H 1.031181 0.623263 0.571863 0.028 Uiso 1 1 calc R U . . .
H39C H 1.093167 0.743759 0.553776 0.028 Uiso 1 1 calc R U . . .
C40 C 0.97274(19) 0.9348(2) 0.57572(16) 0.0175(5) Uani 1 1 d . . . . .
H40A H 1.043132 0.961193 0.575931 0.026 Uiso 1 1 calc R U . . .
H40B H 0.953781 0.988893 0.616520 0.026 Uiso 1 1 calc R U . . .
H40C H 0.917370 0.943469 0.515719 0.026 Uiso 1 1 calc R U . . .
C41 C 1.06089(18) 0.7893(3) 0.70186(15) 0.0202(5) Uani 1 1 d . . . . .
H41A H 1.130144 0.825086 0.705465 0.030 Uiso 1 1 calc R U . . .
H41B H 1.071378 0.700487 0.721907 0.030 Uiso 1 1 calc R U . . .
H41C H 1.033448 0.838814 0.739679 0.030 Uiso 1 1 calc R U . . .
C42 C 0.86928(18) 0.6856(2) 0.23360(15) 0.0186(6) Uani 1 1 d . . . . .
H42 H 0.825268 0.614284 0.206406 0.022 Uiso 1 1 calc R U . . .
C43 C 0.95716(17) 0.7142(4) 0.21204(14) 0.0235(4) Uani 1 1 d . . . . .
H43 H 0.972653 0.664084 0.169933 0.028 Uiso 1 1 calc R U . . .
C44 C 1.0222(2) 0.8169(3) 0.25267(18) 0.0258(5) Uani 1 1 d . . . . .
H44 H 1.083451 0.837683 0.239380 0.031 Uiso 1 1 calc R U . . .
C45 C 0.9968(2) 0.8887(3) 0.31269(18) 0.0243(5) Uani 1 1 d . . . . .
H45 H 1.040463 0.959450 0.341508 0.029 Uiso 1 1 calc R U . . .
C46 C 0.9068(2) 0.8563(2) 0.33042(16) 0.0191(5) Uani 1 1 d . . . . .
H46 H 0.888591 0.906681 0.371006 0.023 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O1 2.0062(15) . ?
Pd1 N1 2.0616(17) . ?
Pd1 O2 2.0107(15) . ?
Pd1 N2 2.0527(19) . ?
O1 C1 1.342(3) . ?
N1 C7 1.500(3) . ?
N1 C8 1.508(3) . ?
N1 C23 1.508(3) . ?
C1 C2 1.422(3) . ?
C1 C6 1.409(3) . ?
O2 C10 1.341(3) . ?
N2 C42 1.341(3) . ?
N2 C46 1.342(3) . ?
C2 C3 1.402(3) . ?
C2 C38 1.538(3) . ?
O3 C31 1.200(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.397(3) . ?
O4 C31 1.341(3) . ?
O4 C32 1.459(3) . ?
C4 C5 1.393(3) . ?
C4 C34 1.538(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(3) . ?
C6 C7 1.497(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.499(3) . ?
C9 C10 1.408(3) . ?
C9 C14 1.391(3) . ?
C10 C11 1.425(3) . ?
C11 C12 1.395(3) . ?
C11 C19 1.537(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.400(4) . ?
C13 C14 1.386(3) . ?
C13 C15 1.537(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.525(4) . ?
C15 C17 1.532(4) . ?
C15 C18 1.533(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.539(3) . ?
C19 C21 1.542(3) . ?
C19 C22 1.541(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 1.0000 . ?
C23 C24 1.535(3) . ?
C23 C31 1.533(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.510(3) . ?
C25 C26 1.389(4) . ?
C25 C30 1.395(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.387(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.388(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.376(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.387(5) . ?
C30 H30 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.507(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.536(3) . ?
C34 C36 1.541(4) . ?
C34 C37 1.533(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.538(3) . ?
C38 C40 1.539(3) . ?
C38 C41 1.535(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42 0.9500 . ?
C42 C43 1.383(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.384(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.379(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.384(4) . ?
C46 H46 0.9500 . ?

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
O1 Pd1 N1 94.00(7) . . ?
O1 Pd1 O2 174.46(6) . . ?
O1 Pd1 N2 86.84(7) . . ?
O2 Pd1 N1 91.51(7) . . ?
O2 Pd1 N2 87.68(7) . . ?
N2 Pd1 N1 177.11(8) . . ?
C1 O1 Pd1 121.84(13) . . ?
C7 N1 Pd1 109.37(12) . . ?
C7 N1 C8 107.03(16) . . ?
C7 N1 C23 113.19(16) . . ?
C8 N1 Pd1 101.96(12) . . ?
C23 N1 Pd1 112.05(13) . . ?
C23 N1 C8 112.56(17) . . ?
O1 C1 C2 121.24(19) . . ?
O1 C1 C6 119.91(18) . . ?
C6 C1 C2 118.76(19) . . ?
C10 O2 Pd1 126.65(14) . . ?
C42 N2 Pd1 119.71(16) . . ?
C42 N2 C46 119.1(2) . . ?
C46 N2 Pd1 121.16(16) . . ?
C1 C2 C38 121.16(19) . . ?
C3 C2 C1 117.61(18) . . ?
C3 C2 C38 121.22(18) . . ?
C2 C3 H3 118.1 . . ?
C4 C3 C2 123.80(18) . . ?
C4 C3 H3 118.1 . . ?
C31 O4 C32 116.88(17) . . ?
C3 C4 C34 123.46(19) . . ?
C5 C4 C3 117.12(19) . . ?
C5 C4 C34 119.39(19) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.32(19) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C7 118.27(18) . . ?
C5 C6 C1 121.22(18) . . ?
C5 C6 C7 120.25(17) . . ?
N1 C7 H7A 108.5 . . ?
N1 C7 H7B 108.5 . . ?
C6 C7 N1 115.25(17) . . ?
C6 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
N1 C8 H8A 108.4 . . ?
N1 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
C9 C8 N1 115.6(2) . . ?
C9 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
C10 C9 C8 122.01(19) . . ?
C14 C9 C8 116.86(19) . . ?
C14 C9 C10 120.9(2) . . ?
O2 C10 C9 122.02(19) . . ?
O2 C10 C11 119.8(2) . . ?
C9 C10 C11 118.2(2) . . ?
C10 C11 C19 121.4(2) . . ?
C12 C11 C10 118.1(2) . . ?
C12 C11 C19 120.5(2) . . ?
C11 C12 H12 117.9 . . ?
C11 C12 C13 124.2(2) . . ?
C13 C12 H12 117.9 . . ?
C12 C13 C15 121.5(2) . . ?
C14 C13 C12 116.3(2) . . ?
C14 C13 C15 122.2(2) . . ?
C9 C14 H14 118.9 . . ?
C13 C14 C9 122.2(2) . . ?
C13 C14 H14 118.9 . . ?
C16 C15 C13 109.1(2) . . ?
C16 C15 C17 109.1(2) . . ?
C16 C15 C18 109.3(2) . . ?
C17 C15 C13 111.2(2) . . ?
C17 C15 C18 107.2(2) . . ?
C18 C15 C13 110.9(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C19 C20 111.14(19) . . ?
C11 C19 C21 112.9(2) . . ?
C11 C19 C22 108.64(19) . . ?
C20 C19 C21 106.1(2) . . ?
C20 C19 C22 110.9(2) . . ?
C22 C19 C21 107.2(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 H23 106.6 . . ?
N1 C23 C24 114.26(17) . . ?
N1 C23 C31 111.73(17) . . ?
C24 C23 H23 106.6 . . ?
C31 C23 H23 106.6 . . ?
C31 C23 C24 110.41(18) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C25 C24 C23 110.79(18) . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C26 C25 C24 119.8(2) . . ?
C26 C25 C30 118.6(2) . . ?
C30 C25 C24 121.5(2) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.6(2) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.9 . . ?
C26 C27 C28 120.3(2) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 H28 120.3 . . ?
C29 C28 C27 119.4(2) . . ?
C29 C28 H28 120.3 . . ?
C28 C29 H29 119.7 . . ?
C28 C29 C30 120.6(3) . . ?
C30 C29 H29 119.7 . . ?
C25 C30 H30 119.8 . . ?
C29 C30 C25 120.4(2) . . ?
C29 C30 H30 119.8 . . ?
O3 C31 O4 124.3(2) . . ?
O3 C31 C23 125.7(2) . . ?
O4 C31 C23 109.99(18) . . ?
O4 C32 H32A 110.5 . . ?
O4 C32 H32B 110.5 . . ?
O4 C32 C33 106.06(18) . . ?
H32A C32 H32B 108.7 . . ?
C33 C32 H32A 110.5 . . ?
C33 C32 H32B 110.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C4 C34 C36 109.76(19) . . ?
C35 C34 C4 109.14(19) . . ?
C35 C34 C36 108.9(2) . . ?
C37 C34 C4 112.46(18) . . ?
C37 C34 C35 108.32(19) . . ?
C37 C34 C36 108.24(18) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C2 C38 C40 110.01(18) . . ?
C39 C38 C2 109.65(19) . . ?
C39 C38 C40 110.2(2) . . ?
C41 C38 C2 112.43(18) . . ?
C41 C38 C39 107.59(18) . . ?
C41 C38 C40 106.96(19) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N2 C42 H42 119.1 . . ?
N2 C42 C43 121.8(2) . . ?
C43 C42 H42 119.1 . . ?
C42 C43 H43 120.5 . . ?
C42 C43 C44 119.1(3) . . ?
C44 C43 H43 120.5 . . ?
C43 C44 H44 120.5 . . ?
C45 C44 C43 119.0(2) . . ?
C45 C44 H44 120.5 . . ?
C44 C45 H45 120.5 . . ?
C44 C45 C46 119.1(2) . . ?
C46 C45 H45 120.5 . . ?
N2 C46 C45 121.8(2) . . ?
N2 C46 H46 119.1 . . ?
C45 C46 H46 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C1 C2 141.53(16) . . . . ?
Pd1 O1 C1 C6 -41.9(3) . . . . ?
Pd1 N1 C7 C6 -59.7(2) . . . . ?
Pd1 N1 C8 C9 73.1(2) . . . . ?
Pd1 N1 C23 C24 43.6(2) . . . . ?
Pd1 N1 C23 C31 169.89(13) . . . . ?
Pd1 O2 C10 C9 -0.1(3) . . . . ?
Pd1 O2 C10 C11 179.64(15) . . . . ?
Pd1 N2 C42 C43 -179.98(19) . . . . ?
Pd1 N2 C46 C45 178.94(19) . . . . ?
O1 C1 C2 C3 -179.3(2) . . . . ?
O1 C1 C2 C38 2.2(3) . . . . ?
O1 C1 C6 C5 179.0(2) . . . . ?
O1 C1 C6 C7 -6.7(3) . . . . ?
N1 C8 C9 C10 -49.5(3) . . . . ?
N1 C8 C9 C14 135.3(2) . . . . ?
N1 C23 C24 C25 -150.89(19) . . . . ?
N1 C23 C31 O3 -111.4(2) . . . . ?
N1 C23 C31 O4 68.3(2) . . . . ?
C1 C2 C3 C4 -1.1(4) . . . . ?
C1 C2 C38 C39 -63.3(3) . . . . ?
C1 C2 C38 C40 58.0(3) . . . . ?
C1 C2 C38 C41 177.0(2) . . . . ?
C1 C6 C7 N1 64.8(3) . . . . ?
O2 C10 C11 C12 179.4(2) . . . . ?
O2 C10 C11 C19 -3.5(3) . . . . ?
N2 C42 C43 C44 1.0(4) . . . . ?
C2 C1 C6 C5 -4.4(4) . . . . ?
C2 C1 C6 C7 169.9(2) . . . . ?
C2 C3 C4 C5 -1.9(4) . . . . ?
C2 C3 C4 C34 -179.8(2) . . . . ?
C3 C2 C38 C39 118.3(3) . . . . ?
C3 C2 C38 C40 -120.4(2) . . . . ?
C3 C2 C38 C41 -1.4(3) . . . . ?
C3 C4 C5 C6 1.7(4) . . . . ?
C3 C4 C34 C35 -121.3(3) . . . . ?
C3 C4 C34 C36 119.4(3) . . . . ?
C3 C4 C34 C37 -1.1(3) . . . . ?
C4 C5 C6 C1 1.4(4) . . . . ?
C4 C5 C6 C7 -172.8(2) . . . . ?
C5 C4 C34 C35 60.8(3) . . . . ?
C5 C4 C34 C36 -58.4(3) . . . . ?
C5 C4 C34 C37 -179.0(2) . . . . ?
C5 C6 C7 N1 -120.9(2) . . . . ?
C6 C1 C2 C3 4.1(3) . . . . ?
C6 C1 C2 C38 -174.3(2) . . . . ?
C7 N1 C8 C9 -172.09(18) . . . . ?
C7 N1 C23 C24 -80.6(2) . . . . ?
C7 N1 C23 C31 45.6(2) . . . . ?
C8 N1 C7 C6 -169.44(18) . . . . ?
C8 N1 C23 C24 157.86(17) . . . . ?
C8 N1 C23 C31 -75.9(2) . . . . ?
C8 C9 C10 O2 5.1(3) . . . . ?
C8 C9 C10 C11 -174.7(2) . . . . ?
C8 C9 C14 C13 174.9(2) . . . . ?
C9 C10 C11 C12 -0.8(3) . . . . ?
C9 C10 C11 C19 176.3(2) . . . . ?
C10 C9 C14 C13 -0.3(3) . . . . ?
C10 C11 C12 C13 1.2(3) . . . . ?
C10 C11 C19 C20 60.7(3) . . . . ?
C10 C11 C19 C21 179.7(2) . . . . ?
C10 C11 C19 C22 -61.6(3) . . . . ?
C11 C12 C13 C14 -1.2(3) . . . . ?
C11 C12 C13 C15 -179.0(2) . . . . ?
C12 C11 C19 C20 -122.3(2) . . . . ?
C12 C11 C19 C21 -3.3(3) . . . . ?
C12 C11 C19 C22 115.4(2) . . . . ?
C12 C13 C14 C9 0.7(3) . . . . ?
C12 C13 C15 C16 84.3(3) . . . . ?
C12 C13 C15 C17 -155.4(3) . . . . ?
C12 C13 C15 C18 -36.2(3) . . . . ?
C14 C9 C10 O2 -179.9(2) . . . . ?
C14 C9 C10 C11 0.3(3) . . . . ?
C14 C13 C15 C16 -93.4(3) . . . . ?
C14 C13 C15 C17 27.0(3) . . . . ?
C14 C13 C15 C18 146.2(3) . . . . ?
C15 C13 C14 C9 178.5(2) . . . . ?
C19 C11 C12 C13 -175.8(2) . . . . ?
C23 N1 C7 C6 66.0(2) . . . . ?
C23 N1 C8 C9 -47.1(2) . . . . ?
C23 C24 C25 C26 62.3(3) . . . . ?
C23 C24 C25 C30 -118.9(2) . . . . ?
C24 C23 C31 O3 17.0(3) . . . . ?
C24 C23 C31 O4 -163.33(18) . . . . ?
C24 C25 C26 C27 177.5(2) . . . . ?
C24 C25 C30 C29 -177.3(3) . . . . ?
C25 C26 C27 C28 0.6(4) . . . . ?
C26 C25 C30 C29 1.6(3) . . . . ?
C26 C27 C28 C29 0.0(4) . . . . ?
C27 C28 C29 C30 0.2(4) . . . . ?
C28 C29 C30 C25 -1.0(4) . . . . ?
C30 C25 C26 C27 -1.4(4) . . . . ?
C31 O4 C32 C33 -166.8(2) . . . . ?
C31 C23 C24 C25 82.2(2) . . . . ?
C32 O4 C31 O3 -0.3(3) . . . . ?
C32 O4 C31 C23 179.98(18) . . . . ?
C34 C4 C5 C6 179.8(2) . . . . ?
C38 C2 C3 C4 177.4(2) . . . . ?
C42 N2 C46 C45 -0.9(4) . . . . ?
C42 C43 C44 C45 -0.8(4) . . . . ?
C43 C44 C45 C46 -0.2(4) . . . . ?
C44 C45 C46 N2 1.1(4) . . . . ?
C46 N2 C42 C43 -0.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.974(4)
2 0.026(4)

####################################################################### 
# 
# 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_8v00077_0m
_database_code_depnum_ccdc_archive 'CCDC 2070850'
loop_
_audit_author_name
_audit_author_address
'Georgina Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-11-10 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2021-11-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H2 Cl2, C22 H29 N O4'
_chemical_formula_sum            'C23 H31 Cl2 N O4'
_chemical_formula_weight         456.39
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.1011(3)
_cell_length_b                   12.1705(2)
_cell_length_c                   17.0857(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.1340(10)
_cell_angle_gamma                90
_cell_volume                     4592.55(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.96
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.912
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0453 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.9628.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42089
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.961
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4380
_reflns_number_total             5056
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5056
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0641P)²+7.7069P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1237
_refine_special_details          ?
_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
 Cl1-Cl2 \\sim Cl1-Cl2A
 with sigma of 0.02
 Cl2A-C1T \\sim Cl1A-C1T \\sim Cl2-C1S \\sim Cl1-C1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1S \\sim C1T: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Others
 Fixed Sof: Cl1(0.9) C1S(0.9) H1SA(0.9) H1SB(0.9) Cl2(0.9) Cl1A(0.1) C1T(0.1)
 H1TA(0.1) H1TB(0.1) Cl2A(0.1)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1T(H1TA,H1TB), C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B), C7(H7A,
 H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C19(H19), C21(H21)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.88562(3) 0.57723(6) 0.74371(4) 0.04132(17) Uani 0.9 1 d D . P A 1
C1S C 0.91558(13) 0.7006(2) 0.78233(14) 0.0345(5) Uani 0.9 1 d D U P A 1
H1SA H 0.882175 0.748113 0.799339 0.041 Uiso 0.9 1 calc R U P A 1
H1SB H 0.937284 0.740133 0.741223 0.041 Uiso 0.9 1 calc R U P A 1
Cl2 Cl 0.96601(3) 0.67368(5) 0.86296(3) 0.03695(16) Uani 0.9 1 d D . P A 1
Cl1A Cl 1.0074(9) 0.6580(16) 0.7019(18) 0.217(14) Uani 0.1 1 d D . P A -1
C1T C 0.9542(11) 0.716(2) 0.764(2) 0.084(10) Uani 0.1 1 d D U P A -1
H1TA H 0.938644 0.785573 0.740627 0.100 Uiso 0.1 1 calc R U P A -1
H1TB H 0.974500 0.734106 0.815082 0.100 Uiso 0.1 1 calc R U P A -1
Cl2A Cl 0.8928(7) 0.6262(10) 0.7793(6) 0.106(4) Uani 0.1 1 d D . P A -1
O1 O 0.74909(5) 0.48713(9) 0.82331(6) 0.0176(2) Uani 1 1 d . . . . .
N1 N 0.68188(6) 0.65716(11) 0.75659(7) 0.0126(3) Uani 1 1 d . . . . .
C1 C 0.72416(7) 0.67006(13) 0.69190(9) 0.0143(3) Uani 1 1 d . . . . .
H1A H 0.763048 0.633742 0.706454 0.017 Uiso 1 1 calc R U . . .
H1B H 0.732313 0.749148 0.683752 0.017 Uiso 1 1 calc R U . . .
O2 O 0.58942(5) 0.51161(10) 0.78345(7) 0.0179(2) Uani 1 1 d . . . . .
H2 H 0.6197(12) 0.534(2) 0.7654(14) 0.033(6) Uiso 1 1 d . . . . .
C2 C 0.71365(7) 0.67529(12) 0.83185(9) 0.0139(3) Uani 1 1 d . . . . .
H2A H 0.683947 0.693221 0.871893 0.017 Uiso 1 1 calc R U . . .
H2B H 0.741500 0.738531 0.827576 0.017 Uiso 1 1 calc R U . . .
O3 O 0.70082(6) 0.43504(10) 0.67010(7) 0.0189(3) Uani 1 1 d . . . . .
H3 H 0.7091(11) 0.460(2) 0.7028(15) 0.027(7) Uiso 1 1 d . . . . .
C3 C 0.74934(7) 0.57440(13) 0.85721(9) 0.0141(3) Uani 1 1 d . . . . .
O4 O 0.78066(5) 0.59534(9) 0.92357(7) 0.0166(2) Uani 1 1 d . . . . .
C5 C 0.81305(7) 0.50319(13) 0.95975(10) 0.0183(3) Uani 1 1 d . . . . .
H5A H 0.841363 0.470782 0.922588 0.022 Uiso 1 1 calc R U . . .
H5B H 0.784183 0.445625 0.975217 0.022 Uiso 1 1 calc R U . . .
C6 C 0.84738(9) 0.54721(15) 1.03079(11) 0.0266(4) Uani 1 1 d . . . . .
H6A H 0.869160 0.486998 1.057498 0.040 Uiso 1 1 calc R U . . .
H6B H 0.818934 0.580398 1.066550 0.040 Uiso 1 1 calc R U . . .
H6C H 0.876404 0.602865 1.014562 0.040 Uiso 1 1 calc R U . . .
C7 C 0.62935(7) 0.73168(13) 0.74577(9) 0.0145(3) Uani 1 1 d . . . . .
H7A H 0.612169 0.723721 0.691730 0.017 Uiso 1 1 calc R U . . .
H7B H 0.643139 0.808605 0.752540 0.017 Uiso 1 1 calc R U . . .
C8 C 0.58053(7) 0.70793(13) 0.80326(9) 0.0141(3) Uani 1 1 d . . . . .
C9 C 0.56223(7) 0.59999(13) 0.81772(9) 0.0147(3) Uani 1 1 d . . . . .
C10 C 0.51534(7) 0.57738(14) 0.86846(9) 0.0175(3) Uani 1 1 d . . . . .
C11 C 0.48733(7) 0.66600(15) 0.90405(9) 0.0198(3) Uani 1 1 d . . . . .
H11 H 0.455534 0.651844 0.938591 0.024 Uiso 1 1 calc R U . . .
C12 C 0.50414(7) 0.77401(15) 0.89093(9) 0.0193(3) Uani 1 1 d . . . . .
C13 C 0.55118(7) 0.79357(14) 0.84023(9) 0.0167(3) Uani 1 1 d . . . . .
H13 H 0.563403 0.867081 0.830796 0.020 Uiso 1 1 calc R U . . .
C14 C 0.49585(8) 0.46103(15) 0.88233(11) 0.0232(4) Uani 1 1 d . . . . .
H14A H 0.465231 0.459863 0.922356 0.035 Uiso 1 1 calc R U . . .
H14B H 0.530932 0.417284 0.900214 0.035 Uiso 1 1 calc R U . . .
H14C H 0.478669 0.430000 0.833455 0.035 Uiso 1 1 calc R U . . .
C15 C 0.47228(9) 0.86841(17) 0.92917(12) 0.0292(4) Uani 1 1 d . . . . .
H15A H 0.441210 0.839667 0.963146 0.044 Uiso 1 1 calc R U . . .
H15B H 0.453191 0.915301 0.888685 0.044 Uiso 1 1 calc R U . . .
H15C H 0.501731 0.911553 0.960514 0.044 Uiso 1 1 calc R U . . .
C16 C 0.69865(7) 0.62096(13) 0.61692(9) 0.0140(3) Uani 1 1 d . . . . .
C17 C 0.68765(7) 0.50791(13) 0.61063(9) 0.0145(3) Uani 1 1 d . . . . .
C18 C 0.66257(7) 0.46338(13) 0.54118(9) 0.0150(3) Uani 1 1 d . . . . .
C19 C 0.64984(7) 0.53341(13) 0.47828(9) 0.0150(3) Uani 1 1 d . . . . .
H19 H 0.632739 0.503365 0.431137 0.018 Uiso 1 1 calc R U . . .
C20 C 0.66125(7) 0.64607(13) 0.48189(9) 0.0148(3) Uani 1 1 d . . . . .
C21 C 0.68548(7) 0.68788(13) 0.55214(9) 0.0145(3) Uani 1 1 d . . . . .
H21 H 0.693302 0.764465 0.556128 0.017 Uiso 1 1 calc R U . . .
C22 C 0.65017(8) 0.34207(13) 0.53465(10) 0.0209(3) Uani 1 1 d . . . . .
H22A H 0.624196 0.327823 0.488014 0.031 Uiso 1 1 calc R U . . .
H22B H 0.629746 0.316987 0.581352 0.031 Uiso 1 1 calc R U . . .
H22C H 0.688488 0.302398 0.530335 0.031 Uiso 1 1 calc R U . . .
C23 C 0.64671(7) 0.71988(14) 0.41293(9) 0.0191(3) Uani 1 1 d . . . . .
H23A H 0.652912 0.679592 0.364214 0.029 Uiso 1 1 calc R U . . .
H23B H 0.673344 0.784266 0.415359 0.029 Uiso 1 1 calc R U . . .
H23C H 0.604426 0.743793 0.414352 0.029 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C1S 1.759(3) . ?
Cl1 Cl2A 0.862(10) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S Cl2 1.770(2) . ?
C1S C1T 0.940(18) . ?
C1S Cl2A 1.037(14) . ?
Cl2 C1T 1.78(4) . ?
Cl2 Cl2A 2.196(13) . ?
Cl1A C1T 1.761(16) . ?
C1T H1TA 0.9900 . ?
C1T H1TB 0.9900 . ?
C1T Cl2A 1.773(16) . ?
O1 C3 1.2097(19) . ?
N1 C1 1.4820(18) . ?
N1 C2 1.4587(18) . ?
N1 C7 1.4792(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C16 1.504(2) . ?
O2 H2 0.80(3) . ?
O2 C9 1.3737(19) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.514(2) . ?
O3 H3 0.66(3) . ?
O3 C17 1.3717(19) . ?
C3 O4 1.3309(19) . ?
O4 C5 1.4557(18) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.506(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.514(2) . ?
C8 C9 1.399(2) . ?
C8 C13 1.392(2) . ?
C9 C10 1.403(2) . ?
C10 C11 1.394(2) . ?
C10 C14 1.501(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.387(3) . ?
C12 C13 1.398(2) . ?
C12 C15 1.509(2) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.401(2) . ?
C16 C21 1.396(2) . ?
C17 C18 1.400(2) . ?
C18 C19 1.392(2) . ?
C18 C22 1.505(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.395(2) . ?
C20 C21 1.392(2) . ?
C20 C23 1.507(2) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
Cl2A Cl1 C1S 24.4(10) . . ?
Cl1 C1S H1SA 109.5 . . ?
Cl1 C1S H1SB 109.5 . . ?
Cl1 C1S Cl2 110.57(14) . . ?
H1SA C1S H1SB 108.1 . . ?
Cl2 C1S H1SA 109.5 . . ?
Cl2 C1S H1SB 109.5 . . ?
C1T C1S Cl1 112.5(17) . . ?
C1T C1S H1SA 132.5 . . ?
C1T C1S H1SB 36.4 . . ?
C1T C1S Cl2 75(3) . . ?
C1T C1S Cl2A 127.3(16) . . ?
Cl2A C1S Cl1 20.0(6) . . ?
Cl2A C1S H1SA 99.1 . . ?
Cl2A C1S H1SB 129.6 . . ?
Cl2A C1S Cl2 99.6(7) . . ?
C1S Cl2 C1T 30.7(7) . . ?
C1S Cl2 Cl2A 27.7(4) . . ?
C1T Cl2 Cl2A 51.7(7) . . ?
C1S C1T Cl2 74(2) . . ?
C1S C1T Cl1A 139(2) . . ?
C1S C1T H1TA 90.0 . . ?
C1S C1T H1TB 97.9 . . ?
C1S C1T Cl2A 27.7(9) . . ?
Cl2 C1T H1TA 131.9 . . ?
Cl2 C1T H1TB 35.0 . . ?
Cl1A C1T Cl2 112(2) . . ?
Cl1A C1T H1TA 109.2 . . ?
Cl1A C1T H1TB 109.2 . . ?
Cl1A C1T Cl2A 111.8(15) . . ?
H1TA C1T H1TB 107.9 . . ?
Cl2A C1T Cl2 76.4(12) . . ?
Cl2A C1T H1TA 109.2 . . ?
Cl2A C1T H1TB 109.2 . . ?
Cl1 Cl2A C1S 135.6(15) . . ?
Cl1 Cl2A Cl2 138.8(12) . . ?
Cl1 Cl2A C1T 116.4(16) . . ?
C1S Cl2A Cl2 52.6(6) . . ?
C1S Cl2A C1T 24.9(8) . . ?
C1T Cl2A Cl2 51.9(14) . . ?
C2 N1 C1 110.19(12) . . ?
C2 N1 C7 111.54(12) . . ?
C7 N1 C1 110.83(12) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C16 111.49(12) . . ?
H1A C1 H1B 108.0 . . ?
C16 C1 H1A 109.3 . . ?
C16 C1 H1B 109.3 . . ?
C9 O2 H2 106.8(18) . . ?
N1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
N1 C2 C3 110.99(12) . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C17 O3 H3 112(2) . . ?
O1 C3 C2 125.59(14) . . ?
O1 C3 O4 124.68(14) . . ?
O4 C3 C2 109.72(13) . . ?
C3 O4 C5 116.50(12) . . ?
O4 C5 H5A 110.3 . . ?
O4 C5 H5B 110.3 . . ?
O4 C5 C6 107.06(13) . . ?
H5A C5 H5B 108.6 . . ?
C6 C5 H5A 110.3 . . ?
C6 C5 H5B 110.3 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
N1 C7 C8 112.14(12) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
C9 C8 C7 120.77(14) . . ?
C13 C8 C7 120.47(14) . . ?
C13 C8 C9 118.70(14) . . ?
O2 C9 C8 121.73(14) . . ?
O2 C9 C10 117.05(14) . . ?
C8 C9 C10 121.22(14) . . ?
C9 C10 C14 120.35(15) . . ?
C11 C10 C9 117.90(15) . . ?
C11 C10 C14 121.74(15) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 C10 122.46(15) . . ?
C12 C11 H11 118.8 . . ?
C11 C12 C13 118.14(15) . . ?
C11 C12 C15 121.30(16) . . ?
C13 C12 C15 120.56(16) . . ?
C8 C13 C12 121.57(15) . . ?
C8 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C1 120.94(14) . . ?
C21 C16 C1 120.26(14) . . ?
C21 C16 C17 118.80(14) . . ?
O3 C17 C16 123.15(14) . . ?
O3 C17 C18 116.36(14) . . ?
C18 C17 C16 120.49(14) . . ?
C17 C18 C22 120.52(14) . . ?
C19 C18 C17 118.66(14) . . ?
C19 C18 C22 120.82(14) . . ?
C18 C19 H19 118.8 . . ?
C18 C19 C20 122.44(14) . . ?
C20 C19 H19 118.8 . . ?
C19 C20 C23 121.23(14) . . ?
C21 C20 C19 117.42(14) . . ?
C21 C20 C23 121.35(15) . . ?
C16 C21 H21 118.9 . . ?
C20 C21 C16 122.17(15) . . ?
C20 C21 H21 118.9 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 C1S Cl2 C1T 108.8(16) . . . . ?
Cl1 C1S Cl2 Cl2A -17.4(7) . . . . ?
Cl1 C1S C1T Cl2 -106.5(10) . . . . ?
Cl1 C1S C1T Cl1A -1(6) . . . . ?
Cl1 C1S C1T Cl2A -15.6(13) . . . . ?
Cl1 C1S Cl2A Cl2 125(2) . . . . ?
Cl1 C1S Cl2A C1T 46(4) . . . . ?
C1S Cl1 Cl2A Cl2 -81(3) . . . . ?
C1S Cl1 Cl2A C1T -20.0(18) . . . . ?
C1S Cl2 C1T Cl1A -137(2) . . . . ?
C1S Cl2 C1T Cl2A -28.6(9) . . . . ?
C1S C1T Cl2A Cl1 146(3) . . . . ?
C1S C1T Cl2A Cl2 -82(3) . . . . ?
Cl2 C1S C1T Cl1A 106(5) . . . . ?
Cl2 C1S C1T Cl2A 91(2) . . . . ?
Cl2 C1S Cl2A Cl1 -125(2) . . . . ?
Cl2 C1S Cl2A C1T -79(3) . . . . ?
Cl2 C1T Cl2A Cl1 -132.8(13) . . . . ?
Cl2 C1T Cl2A C1S 82(3) . . . . ?
Cl1A C1T Cl2A Cl1 -24(3) . . . . ?
Cl1A C1T Cl2A C1S -169(5) . . . . ?
Cl1A C1T Cl2A Cl2 109(3) . . . . ?
C1T C1S Cl2 Cl2A -126.3(16) . . . . ?
C1T C1S Cl2A Cl1 -46(4) . . . . ?
C1T C1S Cl2A Cl2 79(3) . . . . ?
Cl2A Cl1 C1S Cl2 60(2) . . . . ?
Cl2A Cl1 C1S C1T 141(3) . . . . ?
Cl2A C1S Cl2 C1T 126.3(16) . . . . ?
Cl2A C1S C1T Cl2 -91(2) . . . . ?
Cl2A C1S C1T Cl1A 15(7) . . . . ?
Cl2A Cl2 C1T C1S 28.6(9) . . . . ?
Cl2A Cl2 C1T Cl1A -108.3(17) . . . . ?
O1 C3 O4 C5 -4.7(2) . . . . ?
N1 C1 C16 C17 -64.18(18) . . . . ?
N1 C1 C16 C21 115.80(15) . . . . ?
N1 C2 C3 O1 -4.6(2) . . . . ?
N1 C2 C3 O4 176.33(12) . . . . ?
N1 C7 C8 C9 -45.30(19) . . . . ?
N1 C7 C8 C13 137.46(14) . . . . ?
C1 N1 C2 C3 -79.44(15) . . . . ?
C1 N1 C7 C8 170.80(12) . . . . ?
C1 C16 C17 O3 -2.1(2) . . . . ?
C1 C16 C17 C18 178.50(13) . . . . ?
C1 C16 C21 C20 -179.33(14) . . . . ?
O2 C9 C10 C11 179.75(13) . . . . ?
O2 C9 C10 C14 -1.2(2) . . . . ?
C2 N1 C1 C16 163.49(12) . . . . ?
C2 N1 C7 C8 -66.02(16) . . . . ?
C2 C3 O4 C5 174.40(12) . . . . ?
O3 C17 C18 C19 -178.34(13) . . . . ?
O3 C17 C18 C22 1.2(2) . . . . ?
C3 O4 C5 C6 177.10(14) . . . . ?
C7 N1 C1 C16 -72.56(16) . . . . ?
C7 N1 C2 C3 157.02(12) . . . . ?
C7 C8 C9 O2 3.0(2) . . . . ?
C7 C8 C9 C10 -177.39(13) . . . . ?
C7 C8 C13 C12 177.17(14) . . . . ?
C8 C9 C10 C11 0.1(2) . . . . ?
C8 C9 C10 C14 179.19(14) . . . . ?
C9 C8 C13 C12 -0.1(2) . . . . ?
C9 C10 C11 C12 0.1(2) . . . . ?
C10 C11 C12 C13 -0.3(2) . . . . ?
C10 C11 C12 C15 178.91(16) . . . . ?
C11 C12 C13 C8 0.3(2) . . . . ?
C13 C8 C9 O2 -179.70(14) . . . . ?
C13 C8 C9 C10 -0.1(2) . . . . ?
C14 C10 C11 C12 -178.97(15) . . . . ?
C15 C12 C13 C8 -178.89(15) . . . . ?
C16 C17 C18 C19 1.1(2) . . . . ?
C16 C17 C18 C22 -179.39(14) . . . . ?
C17 C16 C21 C20 0.6(2) . . . . ?
C17 C18 C19 C20 0.1(2) . . . . ?
C18 C19 C20 C21 -0.9(2) . . . . ?
C18 C19 C20 C23 -179.73(14) . . . . ?
C19 C20 C21 C16 0.5(2) . . . . ?
C21 C16 C17 O3 177.92(14) . . . . ?
C21 C16 C17 C18 -1.5(2) . . . . ?
C22 C18 C19 C20 -179.37(15) . . . . ?
C23 C20 C21 C16 179.33(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ef124
_database_code_depnum_ccdc_archive 'CCDC 2060200'
loop_
_audit_author_name
_audit_author_address
'Georgina M. Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-02-01 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2020-11-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H3 N, C40 H58 N2 O4 Pd'
_chemical_formula_sum            'C42 H61 N3 O4 Pd'
_chemical_formula_weight         778.33
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   18.1718(8)
_cell_length_b                   11.3807(4)
_cell_length_c                   20.0056(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4137.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3451
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      50.89
_cell_measurement_theta_min      5.05
_shelx_estimated_absorpt_T_max   0.798
_shelx_estimated_absorpt_T_min   0.316
_exptl_absorpt_coefficient_mu    3.940
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1383 before and 0.0621 after correction.
The Ratio of minimum to maximum transmission is 0.5788.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55090
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.162
_diffrn_reflns_theta_min         5.090
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                8315
_reflns_number_total             8373
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.393(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8373
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0305P)²+0.6995P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0516
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.607(5)
 0.393(5)
2. 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
3. Restrained distances
 C21A-C19 = C22-C19 = C22A-C19 = C20-C19 = C20A-C19 = C21-C19
 1.5 with sigma of 0.02
4. Others
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C23(H23)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C26(H26A,H26B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C16(H16), C18(H18), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40)
5.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C20A(H20D,H20E,H20F), C22A(H22D,H22E,H22F), C21A(H21D,H21E,H21F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1S N 0.5267(2) 0.6538(5) 0.2701(3) 0.0924(19) Uani 1 1 d . . . . .
C1S C 0.4692(2) 0.6201(4) 0.28157(19) 0.0448(9) Uani 1 1 d . . . . .
C2S C 0.39697(16) 0.5727(3) 0.29340(15) 0.0353(6) Uani 1 1 d . . . . .
H2SA H 0.371564 0.620754 0.326876 0.053 Uiso 1 1 calc R U . . .
H2SB H 0.401313 0.491858 0.309780 0.053 Uiso 1 1 calc R U . . .
H2SC H 0.368823 0.573281 0.251620 0.053 Uiso 1 1 calc R U . . .
Pd1 Pd 0.48202(2) 0.73432(2) 0.57029(2) 0.01337(5) Uani 1 1 d . . . . .
O1 O 0.55705(8) 0.69162(14) 0.63939(8) 0.0176(3) Uani 1 1 d . . . . .
N1 N 0.46390(10) 0.56323(17) 0.54222(10) 0.0146(4) Uani 1 1 d . . . . .
C1 C 0.59996(12) 0.5973(2) 0.63185(10) 0.0154(4) Uani 1 1 d . . . . .
O2 O 0.41136(9) 0.79612(15) 0.50180(8) 0.0193(3) Uani 1 1 d . . . . .
N2 N 0.49404(11) 0.90315(18) 0.60209(10) 0.0169(4) Uani 1 1 d . . . . .
C2 C 0.67708(12) 0.6027(2) 0.64315(11) 0.0159(4) Uani 1 1 d . . . . .
O3 O 0.45948(12) 0.33571(17) 0.47755(10) 0.0331(4) Uani 1 1 d . . . . .
C3 C 0.71708(11) 0.4979(2) 0.63874(11) 0.0170(4) Uani 1 1 d . . . . .
H3 H 0.768514 0.501031 0.647079 0.020 Uiso 1 1 calc R U . . .
O4 O 0.51374(11) 0.4109(2) 0.38690(11) 0.0315(5) Uani 1 1 d . . . . .
C4 C 0.68622(12) 0.3890(2) 0.62287(11) 0.0175(4) Uani 1 1 d . . . . .
C5 C 0.61099(13) 0.3883(2) 0.60896(11) 0.0178(4) Uani 1 1 d . . . . .
H5 H 0.588072 0.316589 0.596329 0.021 Uiso 1 1 calc R U . . .
C6 C 0.56902(12) 0.4892(2) 0.61309(11) 0.0165(4) Uani 1 1 d . . . . .
C7 C 0.48843(12) 0.4848(2) 0.59909(13) 0.0179(5) Uani 1 1 d . . . . .
H7A H 0.461507 0.507813 0.640062 0.022 Uiso 1 1 calc R U . . .
H7B H 0.474656 0.402714 0.588457 0.022 Uiso 1 1 calc R U . . .
C8 C 0.38176(11) 0.5514(2) 0.53909(12) 0.0170(4) Uani 1 1 d . . . . .
H8A H 0.361218 0.577792 0.582394 0.020 Uiso 1 1 calc R U . . .
H8B H 0.369710 0.466988 0.534193 0.020 Uiso 1 1 calc R U . . .
C9 C 0.34336(11) 0.6176(2) 0.48427(11) 0.0168(4) Uani 1 1 d . . . . .
C10 C 0.35704(13) 0.7376(2) 0.47192(12) 0.0158(4) Uani 1 1 d . . . . .
C11 C 0.31071(12) 0.7972(2) 0.42522(11) 0.0173(4) Uani 1 1 d . . . . .
C12 C 0.32269(13) 0.9278(2) 0.40917(12) 0.0205(5) Uani 1 1 d . . . . .
C13 C 0.26667(15) 0.9751(2) 0.35814(14) 0.0287(6) Uani 1 1 d . . . . .
H13A H 0.270908 0.930730 0.316345 0.043 Uiso 1 1 calc R U . . .
H13B H 0.276654 1.058384 0.349486 0.043 Uiso 1 1 calc R U . . .
H13C H 0.216789 0.966462 0.376090 0.043 Uiso 1 1 calc R U . . .
C14 C 0.31395(14) 1.0017(2) 0.47261(13) 0.0248(5) Uani 1 1 d . . . . .
H14A H 0.262429 1.000093 0.487070 0.037 Uiso 1 1 calc R U . . .
H14B H 0.328588 1.082984 0.463319 0.037 Uiso 1 1 calc R U . . .
H14C H 0.345221 0.969464 0.508044 0.037 Uiso 1 1 calc R U . . .
C15 C 0.39964(15) 0.9436(2) 0.37837(13) 0.0262(5) Uani 1 1 d . . . . .
H15A H 0.436834 0.912308 0.409054 0.039 Uiso 1 1 calc R U . . .
H15B H 0.408923 1.027335 0.370656 0.039 Uiso 1 1 calc R U . . .
H15C H 0.402180 0.901241 0.335783 0.039 Uiso 1 1 calc R U . . .
C16 C 0.25359(16) 0.7342(2) 0.39560(13) 0.0205(5) Uani 1 1 d . . . . .
H16 H 0.221787 0.774868 0.365835 0.025 Uiso 1 1 calc R U . . .
C17 C 0.24022(12) 0.6152(2) 0.40694(12) 0.0210(5) Uani 1 1 d . . . . .
C18 C 0.28682(13) 0.5587(2) 0.45143(12) 0.0197(4) Uani 1 1 d . . . . .
H18 H 0.279932 0.477266 0.459753 0.024 Uiso 1 1 calc R U . . .
C19 C 0.17549(14) 0.5512(3) 0.37400(13) 0.0291(6) Uani 1 1 d D . . . .
C20 C 0.1741(3) 0.5761(4) 0.2980(2) 0.0335(12) Uani 0.657(8) 1 d D . P A 1
H20A H 0.165270 0.659974 0.290359 0.050 Uiso 0.657(8) 1 calc R U P A 1
H20B H 0.134663 0.530204 0.277081 0.050 Uiso 0.657(8) 1 calc R U P A 1
H20C H 0.221469 0.553817 0.278266 0.050 Uiso 0.657(8) 1 calc R U P A 1
C21 C 0.1864(4) 0.4124(5) 0.3766(3) 0.0477(15) Uani 0.657(8) 1 d D . P A 1
H21A H 0.234853 0.392128 0.358385 0.072 Uiso 0.657(8) 1 calc R U P A 1
H21B H 0.147989 0.374161 0.350069 0.072 Uiso 0.657(8) 1 calc R U P A 1
H21C H 0.183235 0.385544 0.423090 0.072 Uiso 0.657(8) 1 calc R U P A 1
C22 C 0.1063(3) 0.5816(9) 0.4051(4) 0.066(3) Uani 0.657(8) 1 d D . P A 1
H22A H 0.109715 0.568733 0.453464 0.100 Uiso 0.657(8) 1 calc R U P A 1
H22B H 0.067024 0.532224 0.386651 0.100 Uiso 0.657(8) 1 calc R U P A 1
H22C H 0.095081 0.664415 0.396371 0.100 Uiso 0.657(8) 1 calc R U P A 1
C23 C 0.49803(13) 0.5419(2) 0.47500(12) 0.0173(4) Uani 1 1 d . . . . .
H23 H 0.470578 0.593611 0.443215 0.021 Uiso 1 1 calc R U . . .
C24 C 0.57858(13) 0.5782(2) 0.46890(13) 0.0238(5) Uani 1 1 d . . . . .
H24A H 0.585899 0.654204 0.490934 0.036 Uiso 1 1 calc R U . . .
H24B H 0.591805 0.584836 0.421558 0.036 Uiso 1 1 calc R U . . .
H24C H 0.609782 0.518860 0.490288 0.036 Uiso 1 1 calc R U . . .
C25 C 0.48709(12) 0.4168(2) 0.44910(13) 0.0214(5) Uani 1 1 d . . . . .
C26 C 0.51333(19) 0.2969(4) 0.35499(19) 0.0400(8) Uani 1 1 d . . . . .
H26A H 0.462329 0.272870 0.344221 0.048 Uiso 1 1 calc R U . . .
H26B H 0.535316 0.237069 0.384856 0.048 Uiso 1 1 calc R U . . .
C27 C 0.5579(2) 0.3088(3) 0.29226(17) 0.0503(9) Uani 1 1 d . . . . .
H27A H 0.532187 0.360354 0.260785 0.076 Uiso 1 1 calc R U . . .
H27B H 0.564676 0.231135 0.271943 0.076 Uiso 1 1 calc R U . . .
H27C H 0.606107 0.342510 0.303066 0.076 Uiso 1 1 calc R U . . .
C28 C 0.72977(14) 0.2736(2) 0.62221(15) 0.0215(5) Uani 1 1 d . . . . .
C29 C 0.81287(14) 0.2946(3) 0.62426(14) 0.0260(5) Uani 1 1 d . . . . .
H29A H 0.827519 0.342228 0.585683 0.039 Uiso 1 1 calc R U . . .
H29B H 0.838601 0.218946 0.622821 0.039 Uiso 1 1 calc R U . . .
H29C H 0.825748 0.336001 0.665583 0.039 Uiso 1 1 calc R U . . .
C30 C 0.70763(15) 0.2004(2) 0.68345(15) 0.0295(6) Uani 1 1 d . . . . .
H30A H 0.735372 0.126605 0.683632 0.044 Uiso 1 1 calc R U . . .
H30B H 0.654817 0.183313 0.681531 0.044 Uiso 1 1 calc R U . . .
H30C H 0.718554 0.244696 0.724285 0.044 Uiso 1 1 calc R U . . .
C31 C 0.71246(15) 0.2037(3) 0.55895(15) 0.0331(7) Uani 1 1 d . . . . .
H31A H 0.725427 0.250510 0.519558 0.050 Uiso 1 1 calc R U . . .
H31B H 0.659830 0.185039 0.557789 0.050 Uiso 1 1 calc R U . . .
H31C H 0.741034 0.130655 0.558918 0.050 Uiso 1 1 calc R U . . .
C32 C 0.71480(14) 0.7204(2) 0.65878(13) 0.0187(5) Uani 1 1 d . . . . .
C33 C 0.79870(14) 0.7080(2) 0.66407(14) 0.0253(5) Uani 1 1 d . . . . .
H33A H 0.810851 0.652902 0.700062 0.038 Uiso 1 1 calc R U . . .
H33B H 0.820498 0.784859 0.673847 0.038 Uiso 1 1 calc R U . . .
H33C H 0.818314 0.678317 0.621678 0.038 Uiso 1 1 calc R U . . .
C34 C 0.69898(13) 0.8089(2) 0.60225(13) 0.0227(5) Uani 1 1 d . . . . .
H34A H 0.718571 0.778384 0.560038 0.034 Uiso 1 1 calc R U . . .
H34B H 0.722580 0.884097 0.612662 0.034 Uiso 1 1 calc R U . . .
H34C H 0.645726 0.820367 0.598123 0.034 Uiso 1 1 calc R U . . .
C35 C 0.68621(16) 0.7685(2) 0.72563(14) 0.0262(6) Uani 1 1 d . . . . .
H35A H 0.632558 0.776465 0.723594 0.039 Uiso 1 1 calc R U . . .
H35B H 0.708371 0.845517 0.734262 0.039 Uiso 1 1 calc R U . . .
H35C H 0.699456 0.714197 0.761697 0.039 Uiso 1 1 calc R U . . .
C36 C 0.48595(10) 0.9946(2) 0.56033(16) 0.0203(6) Uani 1 1 d . . . . .
H36 H 0.479140 0.979655 0.514012 0.024 Uiso 1 1 calc R U . . .
C37 C 0.48718(12) 1.1094(2) 0.58238(15) 0.0247(6) Uani 1 1 d . . . . .
H37 H 0.481894 1.172532 0.551685 0.030 Uiso 1 1 calc R U . . .
C38 C 0.49624(14) 1.1311(2) 0.65001(15) 0.0260(5) Uani 1 1 d . . . . .
H38 H 0.495770 1.209294 0.666676 0.031 Uiso 1 1 calc R U . . .
C39 C 0.50595(14) 1.0374(3) 0.69267(14) 0.0254(5) Uani 1 1 d . . . . .
H39 H 0.512815 1.050195 0.739183 0.030 Uiso 1 1 calc R U . . .
C40 C 0.50559(13) 0.9246(2) 0.66707(13) 0.0213(5) Uani 1 1 d . . . . .
H40 H 0.513771 0.860386 0.696466 0.026 Uiso 1 1 calc R U . . .
C20A C 0.1980(5) 0.4567(12) 0.3377(7) 0.053(4) Uani 0.343(8) 1 d D . P A 2
H20D H 0.229325 0.483264 0.300743 0.080 Uiso 0.343(8) 1 calc R U P A 2
H20E H 0.154965 0.415631 0.319629 0.080 Uiso 0.343(8) 1 calc R U P A 2
H20F H 0.225968 0.403163 0.366419 0.080 Uiso 0.343(8) 1 calc R U P A 2
C22A C 0.1264(6) 0.6423(10) 0.3320(5) 0.051(3) Uani 0.343(8) 1 d D . P A 2
H22D H 0.102019 0.696909 0.362759 0.076 Uiso 0.343(8) 1 calc R U P A 2
H22E H 0.089269 0.599230 0.306392 0.076 Uiso 0.343(8) 1 calc R U P A 2
H22F H 0.158096 0.686511 0.301362 0.076 Uiso 0.343(8) 1 calc R U P A 2
C21A C 0.1201(5) 0.5230(9) 0.4348(5) 0.029(2) Uani 0.343(8) 1 d D . P A 2
H21D H 0.143199 0.466491 0.465249 0.044 Uiso 0.343(8) 1 calc R U P A 2
H21E H 0.074430 0.489534 0.417027 0.044 Uiso 0.343(8) 1 calc R U P A 2
H21F H 0.109075 0.595661 0.459025 0.044 Uiso 0.343(8) 1 calc R U P A 2


_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
N1S C1S 1.136(5) . ?
C1S C2S 1.438(5) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
Pd1 O1 2.0016(16) . ?
Pd1 N1 2.053(2) . ?
Pd1 O2 2.0051(16) . ?
Pd1 N2 2.036(2) . ?
O1 C1 1.335(3) . ?
N1 C7 1.513(3) . ?
N1 C8 1.500(3) . ?
N1 C23 1.501(3) . ?
C1 C2 1.421(3) . ?
C1 C6 1.404(3) . ?
O2 C10 1.332(3) . ?
N2 C36 1.342(4) . ?
N2 C40 1.339(3) . ?
C2 C3 1.400(3) . ?
C2 C32 1.536(3) . ?
O3 C25 1.195(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.397(3) . ?
O4 C25 1.337(3) . ?
O4 C26 1.446(4) . ?
C4 C5 1.395(3) . ?
C4 C28 1.533(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.382(3) . ?
C6 C7 1.492(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.502(3) . ?
C9 C10 1.410(3) . ?
C9 C18 1.391(3) . ?
C10 C11 1.429(3) . ?
C11 C12 1.536(3) . ?
C11 C16 1.394(4) . ?
C12 C13 1.539(3) . ?
C12 C14 1.531(3) . ?
C12 C15 1.539(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C16 C17 1.395(4) . ?
C17 C18 1.387(3) . ?
C17 C19 1.532(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.548(5) . ?
C19 C21 1.593(6) . ?
C19 C22 1.446(6) . ?
C19 C20A 1.361(9) . ?
C19 C22A 1.605(10) . ?
C19 C21A 1.610(9) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 1.0000 . ?
C23 C24 1.526(3) . ?
C23 C25 1.527(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.500(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.529(4) . ?
C28 C30 1.535(4) . ?
C28 C31 1.528(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.535(3) . ?
C32 C34 1.541(3) . ?
C32 C35 1.536(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36 0.9500 . ?
C36 C37 1.380(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.385(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.377(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.382(4) . ?
C40 H40 0.9500 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?

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
N1S C1S C2S 177.0(6) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
O1 Pd1 N1 93.89(7) . . ?
O1 Pd1 O2 173.37(7) . . ?
O1 Pd1 N2 86.57(7) . . ?
O2 Pd1 N1 92.47(7) . . ?
O2 Pd1 N2 87.21(8) . . ?
N2 Pd1 N1 176.22(8) . . ?
C1 O1 Pd1 121.00(13) . . ?
C7 N1 Pd1 107.86(15) . . ?
C8 N1 Pd1 104.85(14) . . ?
C8 N1 C7 105.75(17) . . ?
C8 N1 C23 111.06(18) . . ?
C23 N1 Pd1 109.42(14) . . ?
C23 N1 C7 117.15(19) . . ?
O1 C1 C2 121.6(2) . . ?
O1 C1 C6 120.04(19) . . ?
C6 C1 C2 118.4(2) . . ?
C10 O2 Pd1 127.28(15) . . ?
C36 N2 Pd1 121.68(18) . . ?
C40 N2 Pd1 119.50(17) . . ?
C40 N2 C36 118.7(2) . . ?
C1 C2 C32 120.7(2) . . ?
C3 C2 C1 117.7(2) . . ?
C3 C2 C32 121.59(19) . . ?
C2 C3 H3 117.9 . . ?
C4 C3 C2 124.2(2) . . ?
C4 C3 H3 117.9 . . ?
C25 O4 C26 117.0(3) . . ?
C3 C4 C28 123.7(2) . . ?
C5 C4 C3 116.4(2) . . ?
C5 C4 C28 119.9(2) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.6(2) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C7 118.2(2) . . ?
C5 C6 C1 121.6(2) . . ?
C5 C6 C7 120.2(2) . . ?
N1 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C6 C7 N1 114.23(19) . . ?
C6 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N1 C8 H8A 108.1 . . ?
N1 C8 H8B 108.1 . . ?
N1 C8 C9 116.59(18) . . ?
H8A C8 H8B 107.3 . . ?
C9 C8 H8A 108.1 . . ?
C9 C8 H8B 108.1 . . ?
C10 C9 C8 122.1(2) . . ?
C18 C9 C8 116.5(2) . . ?
C18 C9 C10 120.9(2) . . ?
O2 C10 C9 122.4(2) . . ?
O2 C10 C11 119.5(2) . . ?
C9 C10 C11 118.1(2) . . ?
C10 C11 C12 120.8(2) . . ?
C16 C11 C10 118.2(2) . . ?
C16 C11 C12 121.0(2) . . ?
C11 C12 C13 112.6(2) . . ?
C11 C12 C15 109.0(2) . . ?
C14 C12 C11 110.12(19) . . ?
C14 C12 C13 106.8(2) . . ?
C14 C12 C15 111.2(2) . . ?
C15 C12 C13 107.1(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16 118.0 . . ?
C11 C16 C17 124.1(2) . . ?
C17 C16 H16 118.0 . . ?
C16 C17 C19 121.7(2) . . ?
C18 C17 C16 116.6(2) . . ?
C18 C17 C19 121.6(2) . . ?
C9 C18 H18 119.0 . . ?
C17 C18 C9 122.1(2) . . ?
C17 C18 H18 119.0 . . ?
C17 C19 C20 110.4(2) . . ?
C17 C19 C21 111.2(3) . . ?
C17 C19 C22A 110.1(4) . . ?
C17 C19 C21A 104.5(3) . . ?
C20 C19 C21 102.5(3) . . ?
C22 C19 C17 111.7(3) . . ?
C22 C19 C20 111.4(5) . . ?
C22 C19 C21 109.4(5) . . ?
C20A C19 C17 112.0(5) . . ?
C20A C19 C22A 113.5(8) . . ?
C20A C19 C21A 115.7(8) . . ?
C22A C19 C21A 100.2(6) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 H23 105.6 . . ?
N1 C23 C24 115.10(19) . . ?
N1 C23 C25 113.65(19) . . ?
C24 C23 H23 105.6 . . ?
C24 C23 C25 110.5(2) . . ?
C25 C23 H23 105.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C25 O4 123.8(3) . . ?
O3 C25 C23 127.8(2) . . ?
O4 C25 C23 108.4(2) . . ?
O4 C26 H26A 110.4 . . ?
O4 C26 H26B 110.4 . . ?
O4 C26 C27 106.6(3) . . ?
H26A C26 H26B 108.6 . . ?
C27 C26 H26A 110.4 . . ?
C27 C26 H26B 110.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C4 C28 C30 108.8(2) . . ?
C29 C28 C4 112.1(2) . . ?
C29 C28 C30 108.8(2) . . ?
C31 C28 C4 110.3(2) . . ?
C31 C28 C29 107.9(2) . . ?
C31 C28 C30 108.9(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C2 C32 C34 109.69(19) . . ?
C33 C32 C2 112.2(2) . . ?
C33 C32 C34 107.2(2) . . ?
C33 C32 C35 108.0(2) . . ?
C35 C32 C2 109.7(2) . . ?
C35 C32 C34 110.1(2) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N2 C36 H36 118.9 . . ?
N2 C36 C37 122.2(3) . . ?
C37 C36 H36 118.9 . . ?
C36 C37 H37 120.5 . . ?
C36 C37 C38 118.9(3) . . ?
C38 C37 H37 120.5 . . ?
C37 C38 H38 120.6 . . ?
C39 C38 C37 118.8(2) . . ?
C39 C38 H38 120.6 . . ?
C38 C39 H39 120.4 . . ?
C38 C39 C40 119.3(3) . . ?
C40 C39 H39 120.4 . . ?
N2 C40 C39 122.0(3) . . ?
N2 C40 H40 119.0 . . ?
C39 C40 H40 119.0 . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19 C22A H22D 109.5 . . ?
C19 C22A H22E 109.5 . . ?
C19 C22A H22F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C1 C2 133.38(18) . . . . ?
Pd1 O1 C1 C6 -47.4(3) . . . . ?
Pd1 N1 C7 C6 -65.0(2) . . . . ?
Pd1 N1 C8 C9 68.6(2) . . . . ?
Pd1 N1 C23 C24 51.6(2) . . . . ?
Pd1 N1 C23 C25 -179.50(15) . . . . ?
Pd1 O2 C10 C9 -1.9(3) . . . . ?
Pd1 O2 C10 C11 178.46(16) . . . . ?
Pd1 N2 C36 C37 173.85(16) . . . . ?
Pd1 N2 C40 C39 -172.62(19) . . . . ?
O1 C1 C2 C3 175.5(2) . . . . ?
O1 C1 C2 C32 -5.2(3) . . . . ?
O1 C1 C6 C5 -175.8(2) . . . . ?
O1 C1 C6 C7 2.7(3) . . . . ?
N1 C8 C9 C10 -49.4(3) . . . . ?
N1 C8 C9 C18 138.4(2) . . . . ?
N1 C23 C25 O3 -5.1(4) . . . . ?
N1 C23 C25 O4 174.55(19) . . . . ?
C1 C2 C3 C4 1.1(3) . . . . ?
C1 C2 C32 C33 -175.7(2) . . . . ?
C1 C2 C32 C34 -56.7(3) . . . . ?
C1 C2 C32 C35 64.3(3) . . . . ?
C1 C6 C7 N1 60.8(3) . . . . ?
O2 C10 C11 C12 -0.1(3) . . . . ?
O2 C10 C11 C16 -178.9(2) . . . . ?
N2 C36 C37 C38 -0.7(3) . . . . ?
C2 C1 C6 C5 3.4(3) . . . . ?
C2 C1 C6 C7 -178.0(2) . . . . ?
C2 C3 C4 C5 1.9(3) . . . . ?
C2 C3 C4 C28 -176.3(2) . . . . ?
C3 C2 C32 C33 3.5(3) . . . . ?
C3 C2 C32 C34 122.5(2) . . . . ?
C3 C2 C32 C35 -116.5(2) . . . . ?
C3 C4 C5 C6 -2.3(3) . . . . ?
C3 C4 C28 C29 -13.7(3) . . . . ?
C3 C4 C28 C30 106.7(3) . . . . ?
C3 C4 C28 C31 -133.9(2) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
C4 C5 C6 C7 -178.9(2) . . . . ?
C5 C4 C28 C29 168.3(2) . . . . ?
C5 C4 C28 C30 -71.4(3) . . . . ?
C5 C4 C28 C31 48.1(3) . . . . ?
C5 C6 C7 N1 -120.7(2) . . . . ?
C6 C1 C2 C3 -3.7(3) . . . . ?
C6 C1 C2 C32 175.5(2) . . . . ?
C7 N1 C8 C9 -177.6(2) . . . . ?
C7 N1 C23 C24 -71.5(3) . . . . ?
C7 N1 C23 C25 57.4(3) . . . . ?
C8 N1 C7 C6 -176.8(2) . . . . ?
C8 N1 C23 C24 166.9(2) . . . . ?
C8 N1 C23 C25 -64.2(2) . . . . ?
C8 C9 C10 O2 9.0(3) . . . . ?
C8 C9 C10 C11 -171.3(2) . . . . ?
C8 C9 C18 C17 170.4(2) . . . . ?
C9 C10 C11 C12 -179.7(2) . . . . ?
C9 C10 C11 C16 1.4(3) . . . . ?
C10 C9 C18 C17 -1.9(3) . . . . ?
C10 C11 C12 C13 -179.6(2) . . . . ?
C10 C11 C12 C14 -60.6(3) . . . . ?
C10 C11 C12 C15 61.7(3) . . . . ?
C10 C11 C16 C17 -2.3(4) . . . . ?
C11 C16 C17 C18 1.0(4) . . . . ?
C11 C16 C17 C19 178.7(2) . . . . ?
C12 C11 C16 C17 178.9(2) . . . . ?
C16 C11 C12 C13 -0.8(3) . . . . ?
C16 C11 C12 C14 118.2(2) . . . . ?
C16 C11 C12 C15 -119.5(2) . . . . ?
C16 C17 C18 C9 1.2(3) . . . . ?
C16 C17 C19 C20 49.5(4) . . . . ?
C16 C17 C19 C21 162.5(4) . . . . ?
C16 C17 C19 C22 -75.0(6) . . . . ?
C16 C17 C19 C20A 123.1(9) . . . . ?
C16 C17 C19 C22A -4.1(6) . . . . ?
C16 C17 C19 C21A -110.9(5) . . . . ?
C18 C9 C10 O2 -179.0(2) . . . . ?
C18 C9 C10 C11 0.6(3) . . . . ?
C18 C17 C19 C20 -132.9(3) . . . . ?
C18 C17 C19 C21 -19.9(4) . . . . ?
C18 C17 C19 C22 102.6(6) . . . . ?
C18 C17 C19 C20A -59.3(9) . . . . ?
C18 C17 C19 C22A 173.5(5) . . . . ?
C18 C17 C19 C21A 66.7(5) . . . . ?
C19 C17 C18 C9 -176.6(2) . . . . ?
C23 N1 C7 C6 58.9(3) . . . . ?
C23 N1 C8 C9 -49.5(3) . . . . ?
C24 C23 C25 O3 126.0(3) . . . . ?
C24 C23 C25 O4 -54.3(3) . . . . ?
C25 O4 C26 C27 -169.7(2) . . . . ?
C26 O4 C25 O3 -4.6(4) . . . . ?
C26 O4 C25 C23 175.7(2) . . . . ?
C28 C4 C5 C6 176.0(2) . . . . ?
C32 C2 C3 C4 -178.1(2) . . . . ?
C36 N2 C40 C39 3.1(4) . . . . ?
C36 C37 C38 C39 1.9(4) . . . . ?
C37 C38 C39 C40 -0.7(4) . . . . ?
C38 C39 C40 N2 -1.9(4) . . . . ?
C40 N2 C36 C37 -1.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.607(5)
2 0.393(5)

####################################################################### 
# 
# 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_ef71
_database_code_depnum_ccdc_archive 'CCDC 2060147'
loop_
_audit_author_name
_audit_author_address
'Georgina Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-11-03 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_ef71                
;
PROBLEM: Atom C36             has ADP max/min Ratio .....        3.1 prolat
RESPONSE: disordered CH2Cl2 solvent
;
# Added during the CSD deposition process: Wednesday 03 November 2021 02:52 PM
# end Validation Reply Form

_audit_creation_date             2021-10-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36.66 H59.32 N2 O4 Pd'
_chemical_formula_sum            'C36.66 H59.32 N2 O4 Pd'
_chemical_formula_weight         698.50
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8890(2)
_cell_length_b                   11.7145(3)
_cell_length_c                   15.3877(3)
_cell_angle_alpha                103.1830(10)
_cell_angle_beta                 104.3440(10)
_cell_angle_gamma                99.5060(10)
_cell_volume                     1799.70(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      74.527
_cell_measurement_theta_min      3.089
_shelx_estimated_absorpt_T_max   0.842
_shelx_estimated_absorpt_T_min   0.501
_exptl_absorpt_coefficient_mu    4.456
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1132 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.7623.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             743
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            141515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.759
_diffrn_reflns_theta_min         3.089
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6671
_reflns_number_total             7359
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.245
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7359
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+5.7473P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0900
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H2)=1-FVAR(1)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C31(H31A,H31B), C33(H33A,H33B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C18(H18), C20(H20)
3.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.16913(2) 0.67418(2) 0.29510(2) 0.02787(7) Uani 1 1 d . . . . .
O1 O 0.1028(2) 0.5334(2) 0.17876(15) 0.0308(5) Uani 1 1 d . . . . .
O2 O 0.2142(2) 0.8092(2) 0.41427(15) 0.0304(5) Uani 1 1 d . . . . .
O3 O 0.6160(2) 0.6174(2) 0.33060(16) 0.0321(5) Uani 1 1 d . . . . .
O4 O 0.5615(2) 0.4887(2) 0.41094(16) 0.0311(5) Uani 1 1 d . . . . .
N1 N 0.3615(2) 0.6728(2) 0.30559(17) 0.0242(5) Uani 1 1 d . . . . .
C1 C 0.1751(3) 0.4652(3) 0.1426(2) 0.0262(6) Uani 1 1 d . . . . .
C35 C 0.3074(3) 0.5139(3) 0.1538(2) 0.0252(6) Uani 1 1 d . . . . .
C3 C 0.3824(3) 0.4420(3) 0.1171(2) 0.0256(6) Uani 1 1 d . . . . .
H3 H 0.471630 0.476495 0.126536 0.031 Uiso 1 1 calc R U . . .
C4 C 0.3313(3) 0.3214(3) 0.0672(2) 0.0258(6) Uani 1 1 d . . . . .
C5 C 0.4188(3) 0.2461(3) 0.0289(2) 0.0291(7) Uani 1 1 d . . . . .
C6 C 0.4691(3) 0.2996(3) -0.0418(2) 0.0356(8) Uani 1 1 d . . . . .
H6A H 0.524595 0.251002 -0.066427 0.053 Uiso 1 1 calc R U . . .
H6B H 0.519909 0.382629 -0.010639 0.053 Uiso 1 1 calc R U . . .
H6C H 0.394995 0.299154 -0.093334 0.053 Uiso 1 1 calc R U . . .
C7 C 0.5365(3) 0.2477(3) 0.1089(2) 0.0347(7) Uani 1 1 d . . . . .
H7A H 0.505815 0.214256 0.154725 0.052 Uiso 1 1 calc R U . . .
H7B H 0.587288 0.330858 0.139302 0.052 Uiso 1 1 calc R U . . .
H7C H 0.591438 0.198876 0.083844 0.052 Uiso 1 1 calc R U . . .
C8 C 0.3467(4) 0.1142(3) -0.0207(3) 0.0377(8) Uani 1 1 d . . . . .
H8A H 0.315051 0.077743 0.023316 0.057 Uiso 1 1 calc R U . . .
H8B H 0.406376 0.069839 -0.043835 0.057 Uiso 1 1 calc R U . . .
H8C H 0.272595 0.110770 -0.073445 0.057 Uiso 1 1 calc R U . . .
C9 C 0.1998(3) 0.2756(3) 0.0555(2) 0.0280(7) Uani 1 1 d . . . . .
H9 H 0.162238 0.193707 0.020636 0.034 Uiso 1 1 calc R U . . .
C10 C 0.1203(3) 0.3422(3) 0.0917(2) 0.0284(7) Uani 1 1 d . . . . .
C11 C -0.0229(3) 0.2840(3) 0.0791(2) 0.0345(8) Uani 1 1 d . . . . .
C12 C -0.0632(4) 0.1515(4) 0.0212(3) 0.0507(11) Uani 1 1 d . . . . .
H12A H -0.154709 0.118274 0.014770 0.076 Uiso 1 1 calc R U . . .
H12B H -0.008219 0.105741 0.052596 0.076 Uiso 1 1 calc R U . . .
H12C H -0.052365 0.145705 -0.040948 0.076 Uiso 1 1 calc R U . . .
C13 C -0.0419(3) 0.2858(4) 0.1755(3) 0.0401(9) Uani 1 1 d . . . . .
H13A H -0.004662 0.367145 0.218387 0.060 Uiso 1 1 calc R U . . .
H13B H 0.002125 0.228615 0.200659 0.060 Uiso 1 1 calc R U . . .
H13C H -0.135220 0.262774 0.168791 0.060 Uiso 1 1 calc R U . . .
C14 C -0.1138(3) 0.3509(4) 0.0276(2) 0.0418(9) Uani 1 1 d . . . . .
H14A H -0.091522 0.436069 0.063188 0.063 Uiso 1 1 calc R U . . .
H14B H -0.204511 0.314731 0.021423 0.063 Uiso 1 1 calc R U . . .
H14C H -0.103342 0.344284 -0.034701 0.063 Uiso 1 1 calc R U . . .
C15 C 0.3676(3) 0.6429(3) 0.2062(2) 0.0254(6) Uani 1 1 d . . . . .
H15A H 0.322188 0.694388 0.173255 0.030 Uiso 1 1 calc R U . . .
H15B H 0.459961 0.661793 0.206940 0.030 Uiso 1 1 calc R U . . .
C16 C 0.4399(3) 0.7988(3) 0.3566(2) 0.0268(6) Uani 1 1 d . . . . .
H16A H 0.529749 0.806323 0.351927 0.032 Uiso 1 1 calc R U . . .
H16B H 0.400838 0.856102 0.326754 0.032 Uiso 1 1 calc R U . . .
C17 C 0.4447(3) 0.8310(3) 0.4574(2) 0.0250(6) Uani 1 1 d . . . . .
C18 C 0.5628(3) 0.8519(3) 0.5257(2) 0.0251(6) Uani 1 1 d . . . . .
H18 H 0.639066 0.846088 0.507134 0.030 Uiso 1 1 calc R U . . .
C19 C 0.5728(3) 0.8812(3) 0.6204(2) 0.0252(6) Uani 1 1 d . . . . .
C20 C 0.4586(3) 0.8924(3) 0.6431(2) 0.0269(6) Uani 1 1 d . . . . .
H20 H 0.463560 0.914881 0.707441 0.032 Uiso 1 1 calc R U . . .
C21 C 0.3372(3) 0.8730(3) 0.5778(2) 0.0258(6) Uani 1 1 d . . . . .
C22 C 0.2163(3) 0.8895(3) 0.6097(2) 0.0290(7) Uani 1 1 d . . . . .
C23 C 0.1551(3) 0.9798(3) 0.5665(2) 0.0360(8) Uani 1 1 d . . . . .
H23A H 0.215507 1.059521 0.591796 0.054 Uiso 1 1 calc R U . . .
H23B H 0.073400 0.984282 0.581524 0.054 Uiso 1 1 calc R U . . .
H23C H 0.137327 0.953483 0.498479 0.054 Uiso 1 1 calc R U . . .
C24 C 0.2488(3) 0.9389(3) 0.7161(2) 0.0355(8) Uani 1 1 d . . . . .
H24A H 0.312446 1.016753 0.737533 0.053 Uiso 1 1 calc R U . . .
H24B H 0.285686 0.881941 0.746256 0.053 Uiso 1 1 calc R U . . .
H24C H 0.169200 0.949732 0.732349 0.053 Uiso 1 1 calc R U . . .
C25 C 0.1165(3) 0.7672(3) 0.5800(3) 0.0389(8) Uani 1 1 d . . . . .
H25A H 0.034658 0.780340 0.591566 0.058 Uiso 1 1 calc R U . . .
H25B H 0.151201 0.714782 0.616307 0.058 Uiso 1 1 calc R U . . .
H25C H 0.100179 0.728789 0.513284 0.058 Uiso 1 1 calc R U . . .
C26 C 0.3282(3) 0.8362(3) 0.4810(2) 0.0257(6) Uani 1 1 d . . . . .
C27 C 0.6991(3) 0.8868(3) 0.6944(2) 0.0280(7) Uani 1 1 d . . . . .
C28 C 0.6903(3) 0.7605(3) 0.7089(2) 0.0352(8) Uani 1 1 d . . . . .
H28A H 0.771391 0.759551 0.753688 0.053 Uiso 1 1 calc R U . . .
H28B H 0.677096 0.701179 0.649052 0.053 Uiso 1 1 calc R U . . .
H28C H 0.616837 0.740236 0.733071 0.053 Uiso 1 1 calc R U . . .
C29 C 0.8189(3) 0.9200(4) 0.6621(3) 0.0429(9) Uani 1 1 d . . . . .
H29A H 0.818975 0.995378 0.644530 0.064 Uiso 1 1 calc R U . . .
H29B H 0.816187 0.855390 0.607951 0.064 Uiso 1 1 calc R U . . .
H29C H 0.898190 0.930564 0.712987 0.064 Uiso 1 1 calc R U . . .
C30 C 0.7179(4) 0.9785(4) 0.7881(3) 0.0423(9) Uani 1 1 d . . . . .
H30A H 0.795128 0.973346 0.834555 0.063 Uiso 1 1 calc R U . . .
H30B H 0.640907 0.960706 0.809164 0.063 Uiso 1 1 calc R U . . .
H30C H 0.729803 1.059943 0.780351 0.063 Uiso 1 1 calc R U . . .
C31 C 0.4009(3) 0.5831(3) 0.3537(2) 0.0248(6) Uani 1 1 d . . . . .
H31A H 0.339896 0.503874 0.319558 0.030 Uiso 1 1 calc R U . . .
H31B H 0.391136 0.606182 0.417213 0.030 Uiso 1 1 calc R U . . .
C32 C 0.5391(3) 0.5686(3) 0.3625(2) 0.0257(6) Uani 1 1 d . . . . .
C33 C 0.6842(3) 0.4528(3) 0.4180(3) 0.0337(7) Uani 1 1 d . . . . .
H33A H 0.703785 0.444635 0.357687 0.040 Uiso 1 1 calc R U . . .
H33B H 0.676005 0.373067 0.430541 0.040 Uiso 1 1 calc R U . . .
C34 C 0.7953(3) 0.5433(3) 0.4949(3) 0.0382(8) Uani 1 1 d . . . . .
H34A H 0.807715 0.620821 0.480354 0.057 Uiso 1 1 calc R U . . .
H34B H 0.875352 0.514110 0.499874 0.057 Uiso 1 1 calc R U . . .
H34C H 0.774787 0.553653 0.554331 0.057 Uiso 1 1 calc R U . . .
N2 N -0.0261(3) 0.6864(3) 0.2706(2) 0.0424(8) Uani 1 1 d . . . . .
H2 H -0.032928 0.753962 0.320960 0.051 Uiso 0.340(11) 1 calc R U P A 2
C36 C -0.0667(4) 0.7124(6) 0.1790(4) 0.0786(19) Uani 1 1 d . . . . .
H36A H -0.161203 0.704451 0.159820 0.118 Uiso 1 1 calc R U . . .
H36B H -0.043567 0.655144 0.131996 0.118 Uiso 1 1 calc R U . . .
H36C H -0.022032 0.794763 0.184633 0.118 Uiso 1 1 calc R U . . .
C37 C -0.1121(4) 0.5722(5) 0.2674(4) 0.0615(13) Uani 1 1 d . . . . .
H37A H -0.084766 0.554498 0.327602 0.092 Uiso 1 1 calc R U . . .
H37B H -0.105984 0.506218 0.217681 0.092 Uiso 1 1 calc R U . . .
H37C H -0.202502 0.580437 0.254881 0.092 Uiso 1 1 calc R U . . .
C38 C -0.0581(5) 0.7768(5) 0.3325(4) 0.0346(16) Uani 0.660(11) 1 d . . P A 1
H38A H -0.004861 0.855726 0.338113 0.052 Uiso 0.660(11) 1 calc R U P A 1
H38B H -0.041248 0.761982 0.394072 0.052 Uiso 0.660(11) 1 calc R U P A 1
H38C H -0.150636 0.775727 0.308512 0.052 Uiso 0.660(11) 1 calc R U P A 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 O1 2.016(2) . y
Pd1 O2 2.020(2) . y
Pd1 N1 2.064(2) . y
Pd1 N2 2.100(3) . y
O1 C1 1.337(4) . ?
O2 C26 1.337(4) . ?
O3 C32 1.201(4) . ?
O4 C32 1.339(4) . ?
O4 C33 1.452(4) . ?
N1 C15 1.509(4) . ?
N1 C16 1.499(4) . ?
N1 C31 1.477(4) . ?
C1 C35 1.411(4) . ?
C1 C10 1.420(5) . ?
C35 C3 1.391(4) . ?
C35 C15 1.490(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(4) . ?
C4 C5 1.534(4) . ?
C4 C9 1.395(4) . ?
C5 C6 1.539(4) . ?
C5 C7 1.536(5) . ?
C5 C8 1.533(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9 0.9500 . ?
C9 C10 1.389(5) . ?
C10 C11 1.541(4) . ?
C11 C12 1.532(5) . ?
C11 C13 1.545(5) . ?
C11 C14 1.540(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.496(4) . ?
C17 C18 1.388(4) . ?
C17 C26 1.409(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.391(4) . ?
C19 C20 1.391(4) . ?
C19 C27 1.534(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.395(4) . ?
C21 C22 1.540(4) . ?
C21 C26 1.427(4) . ?
C22 C23 1.529(5) . ?
C22 C24 1.534(4) . ?
C22 C25 1.544(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 C28 1.537(5) . ?
C27 C29 1.531(5) . ?
C27 C30 1.532(5) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.518(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.511(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
N2 H2 1.0000 . ?
N2 C36 1.486(5) . ?
N2 C37 1.485(5) . ?
N2 C38 1.406(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?

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
O1 Pd1 O2 172.98(9) . . y
O1 Pd1 N1 92.67(9) . . y
O1 Pd1 N2 85.70(12) . . y
O2 Pd1 N1 93.71(9) . . y
O2 Pd1 N2 88.33(11) . . y
N1 Pd1 N2 172.57(11) . . y
C1 O1 Pd1 125.82(19) . . ?
C26 O2 Pd1 122.52(19) . . ?
C32 O4 C33 116.5(2) . . ?
C15 N1 Pd1 105.21(17) . . ?
C16 N1 Pd1 106.70(18) . . ?
C16 N1 C15 109.1(2) . . ?
C31 N1 Pd1 109.91(17) . . ?
C31 N1 C15 112.6(2) . . ?
C31 N1 C16 112.9(2) . . ?
O1 C1 C35 120.8(3) . . ?
O1 C1 C10 120.8(3) . . ?
C35 C1 C10 118.4(3) . . ?
C1 C35 C15 119.8(3) . . ?
C3 C35 C1 120.5(3) . . ?
C3 C35 C15 119.7(3) . . ?
C35 C3 H3 118.9 . . ?
C4 C3 C35 122.3(3) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C5 120.1(3) . . ?
C3 C4 C9 116.4(3) . . ?
C9 C4 C5 123.6(3) . . ?
C4 C5 C6 109.7(3) . . ?
C4 C5 C7 110.0(3) . . ?
C7 C5 C6 108.6(3) . . ?
C8 C5 C4 112.5(3) . . ?
C8 C5 C6 108.0(3) . . ?
C8 C5 C7 108.0(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9 117.9 . . ?
C10 C9 C4 124.1(3) . . ?
C10 C9 H9 117.9 . . ?
C1 C10 C11 120.4(3) . . ?
C9 C10 C1 118.4(3) . . ?
C9 C10 C11 121.2(3) . . ?
C10 C11 C13 109.6(3) . . ?
C12 C11 C10 112.2(3) . . ?
C12 C11 C13 106.5(3) . . ?
C12 C11 C14 107.2(3) . . ?
C14 C11 C10 110.1(3) . . ?
C14 C11 C13 111.3(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.0 . . ?
N1 C15 H15B 109.0 . . ?
C35 C15 N1 112.8(2) . . ?
C35 C15 H15A 109.0 . . ?
C35 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
N1 C16 H16A 109.3 . . ?
N1 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 N1 111.6(2) . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 C26 121.3(3) . . ?
C26 C17 C16 119.2(3) . . ?
C17 C18 H18 119.0 . . ?
C17 C18 C19 121.9(3) . . ?
C19 C18 H18 119.0 . . ?
C18 C19 C20 116.2(3) . . ?
C18 C19 C27 121.5(3) . . ?
C20 C19 C27 121.9(3) . . ?
C19 C20 H20 117.8 . . ?
C19 C20 C21 124.5(3) . . ?
C21 C20 H20 117.8 . . ?
C20 C21 C22 120.8(3) . . ?
C20 C21 C26 118.1(3) . . ?
C26 C21 C22 121.1(3) . . ?
C21 C22 C25 110.1(3) . . ?
C23 C22 C21 109.4(3) . . ?
C23 C22 C24 107.0(3) . . ?
C23 C22 C25 110.3(3) . . ?
C24 C22 C21 112.8(3) . . ?
C24 C22 C25 107.2(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O2 C26 C17 120.6(3) . . ?
O2 C26 C21 121.7(3) . . ?
C17 C26 C21 117.7(3) . . ?
C19 C27 C28 107.1(3) . . ?
C29 C27 C19 111.4(3) . . ?
C29 C27 C28 108.8(3) . . ?
C29 C27 C30 108.0(3) . . ?
C30 C27 C19 112.5(3) . . ?
C30 C27 C28 109.0(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N1 C31 H31A 108.4 . . ?
N1 C31 H31B 108.4 . . ?
N1 C31 C32 115.6(2) . . ?
H31A C31 H31B 107.4 . . ?
C32 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
O3 C32 O4 124.7(3) . . ?
O3 C32 C31 126.9(3) . . ?
O4 C32 C31 108.3(2) . . ?
O4 C33 H33A 109.3 . . ?
O4 C33 H33B 109.3 . . ?
O4 C33 C34 111.7(3) . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Pd1 N2 H2 109.6 . . ?
C36 N2 Pd1 107.1(2) . . ?
C36 N2 H2 109.6 . . ?
C37 N2 Pd1 111.5(2) . . ?
C37 N2 H2 109.6 . . ?
C37 N2 C36 109.4(4) . . ?
C38 N2 Pd1 119.3(3) . . ?
C38 N2 C36 104.3(4) . . ?
C38 N2 C37 104.7(4) . . ?
N2 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
N2 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 H37A 109.5 . . ?
N2 C37 H37B 109.5 . . ?
N2 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N2 C38 H38A 109.5 . . ?
N2 C38 H38B 109.5 . . ?
N2 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C1 C35 -30.1(4) . . . . ?
Pd1 O1 C1 C10 150.2(2) . . . . ?
Pd1 O2 C26 C17 38.5(4) . . . . ?
Pd1 O2 C26 C21 -142.7(2) . . . . ?
Pd1 N1 C15 C35 -73.5(3) . . . . ?
Pd1 N1 C16 C17 70.5(3) . . . . ?
Pd1 N1 C31 C32 177.4(2) . . . . ?
O1 C1 C35 C3 179.1(3) . . . . ?
O1 C1 C35 C15 -0.1(4) . . . . ?
O1 C1 C10 C9 179.9(3) . . . . ?
O1 C1 C10 C11 -1.5(4) . . . . ?
N1 C16 C17 C18 114.1(3) . . . . ?
N1 C16 C17 C26 -64.1(4) . . . . ?
N1 C31 C32 O3 -4.1(5) . . . . ?
N1 C31 C32 O4 177.3(3) . . . . ?
C1 C35 C3 C4 1.1(5) . . . . ?
C1 C35 C15 N1 59.0(4) . . . . ?
C1 C10 C11 C12 179.3(3) . . . . ?
C1 C10 C11 C13 -62.6(4) . . . . ?
C1 C10 C11 C14 60.0(4) . . . . ?
C35 C1 C10 C9 0.2(4) . . . . ?
C35 C1 C10 C11 178.9(3) . . . . ?
C35 C3 C4 C5 -179.6(3) . . . . ?
C35 C3 C4 C9 0.0(4) . . . . ?
C3 C35 C15 N1 -120.2(3) . . . . ?
C3 C4 C5 C6 -62.1(4) . . . . ?
C3 C4 C5 C7 57.3(4) . . . . ?
C3 C4 C5 C8 177.7(3) . . . . ?
C3 C4 C9 C10 -1.1(5) . . . . ?
C4 C9 C10 C1 1.0(5) . . . . ?
C4 C9 C10 C11 -177.6(3) . . . . ?
C5 C4 C9 C10 178.5(3) . . . . ?
C9 C4 C5 C6 118.3(3) . . . . ?
C9 C4 C5 C7 -122.3(3) . . . . ?
C9 C4 C5 C8 -1.9(4) . . . . ?
C9 C10 C11 C12 -2.0(4) . . . . ?
C9 C10 C11 C13 116.0(3) . . . . ?
C9 C10 C11 C14 -121.3(3) . . . . ?
C10 C1 C35 C3 -1.3(4) . . . . ?
C10 C1 C35 C15 179.6(3) . . . . ?
C15 N1 C16 C17 -176.3(2) . . . . ?
C15 N1 C31 C32 60.5(3) . . . . ?
C15 C35 C3 C4 -179.7(3) . . . . ?
C16 N1 C15 C35 172.3(2) . . . . ?
C16 N1 C31 C32 -63.6(3) . . . . ?
C16 C17 C18 C19 -179.5(3) . . . . ?
C16 C17 C26 O2 2.0(5) . . . . ?
C16 C17 C26 C21 -176.9(3) . . . . ?
C17 C18 C19 C20 -2.1(5) . . . . ?
C17 C18 C19 C27 171.3(3) . . . . ?
C18 C17 C26 O2 -176.2(3) . . . . ?
C18 C17 C26 C21 4.9(5) . . . . ?
C18 C19 C20 C21 1.9(5) . . . . ?
C18 C19 C27 C28 -90.4(3) . . . . ?
C18 C19 C27 C29 28.5(4) . . . . ?
C18 C19 C27 C30 149.9(3) . . . . ?
C19 C20 C21 C22 -179.1(3) . . . . ?
C19 C20 C21 C26 1.6(5) . . . . ?
C20 C19 C27 C28 82.7(4) . . . . ?
C20 C19 C27 C29 -158.5(3) . . . . ?
C20 C19 C27 C30 -37.1(4) . . . . ?
C20 C21 C22 C23 124.3(3) . . . . ?
C20 C21 C22 C24 5.3(4) . . . . ?
C20 C21 C22 C25 -114.4(3) . . . . ?
C20 C21 C26 O2 176.2(3) . . . . ?
C20 C21 C26 C17 -5.0(4) . . . . ?
C22 C21 C26 O2 -3.1(5) . . . . ?
C22 C21 C26 C17 175.8(3) . . . . ?
C26 C17 C18 C19 -1.3(5) . . . . ?
C26 C21 C22 C23 -56.4(4) . . . . ?
C26 C21 C22 C24 -175.5(3) . . . . ?
C26 C21 C22 C25 64.9(4) . . . . ?
C27 C19 C20 C21 -171.5(3) . . . . ?
C31 N1 C15 C35 46.1(3) . . . . ?
C31 N1 C16 C17 -50.4(3) . . . . ?
C32 O4 C33 C34 82.2(4) . . . . ?
C33 O4 C32 O3 -5.1(5) . . . . ?
C33 O4 C32 C31 173.5(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ef89
_database_code_depnum_ccdc_archive 'CCDC 2063653'
loop_
_audit_author_name
_audit_author_address
'Georgina M. Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-02-18 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_audit_creation_date             2021-02-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H66 N2 O4 Pd'
_chemical_formula_sum            'C40 H66 N2 O4 Pd'
_chemical_formula_weight         745.34
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 n 1'
_space_group_name_Hall           'P -2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   9.9356(4)
_cell_length_b                   26.4605(11)
_cell_length_c                   15.5658(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.0420(10)
_cell_angle_gamma                90
_cell_volume                     3952.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9337
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.357
_cell_measurement_theta_min      3.078
_shelx_estimated_absorpt_T_max   0.905
_shelx_estimated_absorpt_T_min   0.862
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0582 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.9143.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            146440
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         2.677
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                15237
_reflns_number_total             15877
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 
;
 Flack x determined using 6940 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.084(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         15877
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0293
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0226P)²+3.7935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0656
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13A-C12 = C15-C12 = C15A-C12 = C14-C12 = C14A-C12
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14A) = Uanis(C15)
4. Others
 Sof(HU)=Sof(HV)=Sof(C20A)=Sof(H8DA)=Sof(H9DA)=Sof(H0EA)=1-FVAR(1)
 Sof(HW)=Sof(HX)=Sof(C20)=Sof(HY)=Sof(HZ)=Sof(H0AA)=FVAR(1)
 Sof(C15A)=Sof(H1EA)=Sof(H2EA)=Sof(H3EA)=Sof(C14A)=Sof(H7EA)=Sof(H8EA)=
 Sof(H9EA)=1-FVAR(2)
 Sof(C14)=Sof(HM)=Sof(HN)=Sof(HO)=Sof(C15)=Sof(HP)=Sof(HQ)=Sof(HR)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H,HA), C16(HS,HT), C19(HU,HV), C19(HW,HX), C21(H1AA,H2AA), C36(H3CA,H4CA),
 C38(H8CA,H9CA), C40(H3DA,H4DA), C1'(H1'A,H1'B), C16'(H16A,H16B), C19'(H19A,
 H19B), C21'(H21A,H21B), C36'(H36A,H36B), C38'(H38A,H38B), C40'(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(HB), C7(HC), C25(H3AA), C27(H4AA), C5'(H5'), C7'(H7'), C25'(H25'),
 C27'(H27')
5.c Idealised Me refined as rotating group:
 C9(HD,HE,HF), C10(HG,HH,HI), C11(HJ,HK,HL), C14(HM,HN,HO), C15(HP,HQ,HR),
 C20(HY,HZ,H0AA), C29(H5AA,H6AA,H7AA), C30(H8AA,H9AA,H0BA), C31(H1BA,H2BA,H3BA),
  C33(H4BA,H5BA,H6BA), C34(H7BA,H8BA,H9BA), C35(H0CA,H1CA,H2CA), C37(H5CA,H6CA,
 H7CA), C39(H0DA,H1DA,H2DA), C41(H5DA,H6DA,H7DA), C9'(H9'A,H9'B,H9'C),
 C10'(H10A,H10B,H10C), C11'(H11A,H11B,H11C), C13'(H13A,H13B,H13C), C14'(H14A,
 H14B,H14C), C15'(H15A,H15B,H15C), C20'(H20A,H20B,H20C), C29'(H29A,H29B,H29C),
 C30'(H30A,H30B,H30C), C31'(H31A,H31B,H31C), C33'(H33A,H33B,H33C), C34'(H34A,
 H34B,H34C), C35'(H35A,H35B,H35C), C37'(H37A,H37B,H37C), C39'(H39A,H39B,H39C),
 C41'(H41A,H41B,H41C), C20A(H8DA,H9DA,H0EA), C15A(H1EA,H2EA,H3EA), C13A(H4EA,
 H5EA,H6EA), C14A(H7EA,H8EA,H9EA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.63612(2) 0.94488(2) 0.42967(2) 0.01655(9) Uani 1 1 d . . . . .
O1 O 0.6035(4) 0.95106(12) 0.5523(3) 0.0228(8) Uani 1 1 d . . . . .
N2 N 0.4792(3) 1.00078(12) 0.3840(2) 0.0179(7) Uani 1 1 d . . . . .
C1 C 0.8747(4) 0.91541(16) 0.5701(3) 0.0241(9) Uani 1 1 d . . . . .
H H 0.9698 0.9013 0.5910 0.029 Uiso 1 1 calc R . . . .
HA H 0.8818 0.9527 0.5748 0.029 Uiso 1 1 calc R . . . .
O2 O 0.6467(4) 0.94066(10) 0.3020(3) 0.0199(8) Uani 1 1 d . . . . .
N1 N 0.8145(3) 0.90096(12) 0.4744(2) 0.0181(7) Uani 1 1 d . . . . .
C2 C 0.7869(4) 0.89644(15) 0.6287(3) 0.0231(8) Uani 1 1 d . . . . .
C3 C 0.6535(4) 0.91785(14) 0.6177(3) 0.0221(8) Uani 1 1 d . . . . .
C4 C 0.5763(5) 0.90409(18) 0.6793(3) 0.0272(10) Uani 1 1 d . . . . .
C5 C 0.6301(5) 0.86652(17) 0.7411(3) 0.0314(10) Uani 1 1 d . . . . .
HB H 0.5771 0.8568 0.7811 0.038 Uiso 1 1 calc R . . . .
C6 C 0.7575(5) 0.84207(17) 0.7482(3) 0.0321(10) Uani 1 1 d . . . . .
C7 C 0.8355(5) 0.85895(16) 0.6911(3) 0.0274(10) Uani 1 1 d . . . . .
HC H 0.9243 0.8443 0.6952 0.033 Uiso 1 1 calc R . . . .
C8 C 0.4381(5) 0.93017(19) 0.6799(3) 0.0337(10) Uani 1 1 d . . . . .
C9 C 0.3262(5) 0.9172(2) 0.5935(3) 0.0388(11) Uani 1 1 d . . . . .
HD H 0.2445 0.9388 0.5886 0.058 Uiso 1 1 calc GR . . . .
HE H 0.2990 0.8817 0.5949 0.058 Uiso 1 1 calc GR . . . .
HF H 0.3643 0.9230 0.5422 0.058 Uiso 1 1 calc GR . . . .
C10 C 0.4616(5) 0.9876(2) 0.6895(3) 0.0377(11) Uani 1 1 d . . . . .
HG H 0.4989 1.0000 0.6410 0.057 Uiso 1 1 calc GR . . . .
HH H 0.5281 0.9949 0.7467 0.057 Uiso 1 1 calc GR . . . .
HI H 0.3729 1.0045 0.6870 0.057 Uiso 1 1 calc GR . . . .
C11 C 0.3796(6) 0.9131(3) 0.7573(4) 0.0523(15) Uani 1 1 d . . . . .
HJ H 0.4497 0.9186 0.8137 0.078 Uiso 1 1 calc GR . . . .
HK H 0.3560 0.8771 0.7507 0.078 Uiso 1 1 calc GR . . . .
HL H 0.2957 0.9327 0.7569 0.078 Uiso 1 1 calc GR . . . .
C12 C 0.8063(7) 0.7981(2) 0.8119(3) 0.0521(16) Uani 1 1 d D . . . .
C14 C 0.9495(10) 0.7927(5) 0.8465(7) 0.037(2) Uani 0.598(13) 1 d D . P A 1
HM H 0.9939 0.7881 0.7977 0.055 Uiso 0.598(13) 1 calc GR . P A 1
HN H 0.9682 0.7631 0.8858 0.055 Uiso 0.598(13) 1 calc GR . P A 1
HO H 0.9871 0.8230 0.8804 0.055 Uiso 0.598(13) 1 calc GR . P A 1
C15 C 0.7316(10) 0.7477(3) 0.7625(5) 0.0321(18) Uani 0.598(13) 1 d D . P A 1
HP H 0.6305 0.7529 0.7440 0.048 Uiso 0.598(13) 1 calc GR . P A 1
HQ H 0.7532 0.7190 0.8036 0.048 Uiso 0.598(13) 1 calc GR . P A 1
HR H 0.7660 0.7408 0.7101 0.048 Uiso 0.598(13) 1 calc GR . P A 1
C16 C 0.7879(4) 0.84582(14) 0.4656(3) 0.0197(8) Uani 1 1 d . . . . .
HS H 0.7456 0.8380 0.4021 0.024 Uiso 1 1 calc R . . . .
HT H 0.7190 0.8368 0.4990 0.024 Uiso 1 1 calc R . . . .
O3 O 1.0362(3) 0.82621(13) 0.5136(3) 0.0406(8) Uani 1 1 d . . . . .
C17 C 0.9166(5) 0.81273(16) 0.4986(3) 0.0258(9) Uani 1 1 d . . . . .
O4 O 0.8759(4) 0.76588(12) 0.5100(3) 0.0423(9) Uani 1 1 d . . . . .
C19 C 0.9886(7) 0.7285(2) 0.5361(5) 0.0648(19) Uani 1 1 d . . . . .
HU H 0.9536 0.6949 0.5120 0.078 Uiso 0.539(12) 1 calc R . P B 2
HV H 1.0659 0.7380 0.5101 0.078 Uiso 0.539(12) 1 calc R . P B 2
HW H 1.0252 0.7209 0.4841 0.078 Uiso 0.461(12) 1 calc R . P B 1
HX H 1.0655 0.7433 0.5830 0.078 Uiso 0.461(12) 1 calc R . P B 1
C20 C 0.9473(11) 0.6846(4) 0.5669(7) 0.034(3) Uani 0.461(12) 1 d . . P B 1
HY H 0.8931 0.6922 0.6096 0.050 Uiso 0.461(12) 1 calc GR . P B 1
HZ H 1.0295 0.6646 0.5962 0.050 Uiso 0.461(12) 1 calc GR . P B 1
H0AA H 0.8897 0.6653 0.5170 0.050 Uiso 0.461(12) 1 calc GR . P B 1
C21 C 0.9102(4) 0.91931(15) 0.4192(3) 0.0207(8) Uani 1 1 d . . . . .
H1AA H 0.9078 0.9567 0.4165 0.025 Uiso 1 1 calc R . . . .
H2AA H 1.0070 0.9088 0.4479 0.025 Uiso 1 1 calc R . . . .
C22 C 0.8667(4) 0.89825(15) 0.3269(3) 0.0197(8) Uani 1 1 d . . . . .
C23 C 0.7325(4) 0.90986(14) 0.2733(3) 0.0183(8) Uani 1 1 d . . . . .
C24 C 0.6905(4) 0.88783(15) 0.1867(3) 0.0187(9) Uani 1 1 d . . . . .
C25 C 0.7850(4) 0.85665(14) 0.1599(3) 0.0185(8) Uani 1 1 d . . . . .
H3AA H 0.7578 0.8428 0.1017 0.022 Uiso 1 1 calc R . . . .
C26 C 0.9173(4) 0.84452(14) 0.2132(3) 0.0197(8) Uani 1 1 d . . . . .
C27 C 0.9554(4) 0.86586(14) 0.2969(3) 0.0194(8) Uani 1 1 d . . . . .
H4AA H 1.0443 0.8583 0.3351 0.023 Uiso 1 1 calc R . . . .
C28 C 0.5451(4) 0.89746(14) 0.1258(3) 0.0195(8) Uani 1 1 d . . . . .
C29 C 0.4347(4) 0.87842(16) 0.1720(3) 0.0261(9) Uani 1 1 d . . . . .
H5AA H 0.3424 0.8905 0.1392 0.039 Uiso 1 1 calc GR . . . .
H6AA H 0.4566 0.8913 0.2331 0.039 Uiso 1 1 calc GR . . . .
H7AA H 0.4351 0.8414 0.1730 0.039 Uiso 1 1 calc GR . . . .
C30 C 0.5265(4) 0.95446(15) 0.1050(3) 0.0259(9) Uani 1 1 d . . . . .
H8AA H 0.5920 0.9651 0.0710 0.039 Uiso 1 1 calc GR . . . .
H9AA H 0.5449 0.9735 0.1608 0.039 Uiso 1 1 calc GR . . . .
H0BA H 0.4309 0.9609 0.0700 0.039 Uiso 1 1 calc GR . . . .
C31 C 0.5188(4) 0.86948(16) 0.0364(3) 0.0263(9) Uani 1 1 d . . . . .
H1BA H 0.5862 0.8809 0.0044 0.039 Uiso 1 1 calc GR . . . .
H2BA H 0.4241 0.8767 0.0006 0.039 Uiso 1 1 calc GR . . . .
H3BA H 0.5293 0.8330 0.0472 0.039 Uiso 1 1 calc GR . . . .
C32 C 1.0126(4) 0.81022(16) 0.1760(3) 0.0241(8) Uani 1 1 d . . . . .
C33 C 0.9355(5) 0.76156(16) 0.1379(3) 0.0311(10) Uani 1 1 d . . . . .
H4BA H 0.9149 0.7418 0.1862 0.047 Uiso 1 1 calc GR . . . .
H5BA H 0.9943 0.7416 0.1090 0.047 Uiso 1 1 calc GR . . . .
H6BA H 0.8483 0.7703 0.0943 0.047 Uiso 1 1 calc GR . . . .
C34 C 1.1465(5) 0.79641(19) 0.2460(3) 0.0353(11) Uani 1 1 d . . . . .
H7BA H 1.1985 0.8273 0.2682 0.053 Uiso 1 1 calc GR . . . .
H8BA H 1.2039 0.7744 0.2192 0.053 Uiso 1 1 calc GR . . . .
H9BA H 1.1230 0.7787 0.2954 0.053 Uiso 1 1 calc GR . . . .
C35 C 1.0545(4) 0.83868(18) 0.1002(3) 0.0310(10) Uani 1 1 d . . . . .
H0CA H 0.9711 0.8456 0.0521 0.047 Uiso 1 1 calc GR . . . .
H1CA H 1.1192 0.8178 0.0775 0.047 Uiso 1 1 calc GR . . . .
H2CA H 1.0999 0.8706 0.1231 0.047 Uiso 1 1 calc GR . . . .
C36 C 0.5469(4) 1.04309(14) 0.3471(3) 0.0212(8) Uani 1 1 d . . . . .
H3CA H 0.4755 1.0689 0.3219 0.025 Uiso 1 1 calc R . . . .
H4CA H 0.5828 1.0298 0.2978 0.025 Uiso 1 1 calc R . . . .
C37 C 0.6660(5) 1.06825(16) 0.4149(3) 0.0300(10) Uani 1 1 d . . . . .
H5CA H 0.6322 1.0807 0.4648 0.045 Uiso 1 1 calc GR . . . .
H6CA H 0.7018 1.0966 0.3869 0.045 Uiso 1 1 calc GR . . . .
H7CA H 0.7408 1.0436 0.4368 0.045 Uiso 1 1 calc GR . . . .
C38 C 0.3626(4) 0.98186(14) 0.3090(3) 0.0199(8) Uani 1 1 d . . . . .
H8CA H 0.4019 0.9700 0.2603 0.024 Uiso 1 1 calc R . . . .
H9CA H 0.2988 1.0103 0.2857 0.024 Uiso 1 1 calc R . . . .
C39 C 0.2798(4) 0.93938(16) 0.3354(3) 0.0280(9) Uani 1 1 d . . . . .
H0DA H 0.3437 0.9132 0.3669 0.042 Uiso 1 1 calc GR . . . .
H1DA H 0.2170 0.9248 0.2820 0.042 Uiso 1 1 calc GR . . . .
H2DA H 0.2250 0.9526 0.3745 0.042 Uiso 1 1 calc GR . . . .
C40 C 0.4235(5) 1.02074(17) 0.4586(3) 0.0291(9) Uani 1 1 d . . . . .
H3DA H 0.5026 1.0349 0.5048 0.035 Uiso 1 1 calc R . . . .
H4DA H 0.3859 0.9919 0.4856 0.035 Uiso 1 1 calc R . . . .
C41 C 0.3096(5) 1.06144(18) 0.4338(4) 0.0374(11) Uani 1 1 d . . . . .
H5DA H 0.3422 1.0892 0.4026 0.056 Uiso 1 1 calc GR . . . .
H6DA H 0.2889 1.0744 0.4879 0.056 Uiso 1 1 calc GR . . . .
H7DA H 0.2251 1.0467 0.3949 0.056 Uiso 1 1 calc GR . . . .
Pd1' Pd 0.20544(2) 0.55156(2) 0.51197(2) 0.01591(8) Uani 1 1 d . . . . .
O1' O 0.2192(4) 0.55552(10) 0.3842(3) 0.0194(8) Uani 1 1 d . . . . .
N2' N 0.0481(3) 0.49573(12) 0.4652(2) 0.0176(7) Uani 1 1 d . . . . .
C1' C 0.4779(4) 0.58177(14) 0.5036(3) 0.0167(7) Uani 1 1 d . . . . .
H1'A H 0.5713 0.5952 0.5335 0.020 Uiso 1 1 calc R . . . .
H1'B H 0.4837 0.5444 0.5045 0.020 Uiso 1 1 calc R . . . .
O2' O 0.1716(4) 0.54771(12) 0.6349(3) 0.0251(8) Uani 1 1 d . . . . .
N1' N 0.3748(3) 0.59854(12) 0.5539(2) 0.0149(6) Uani 1 1 d . . . . .
C2' C 0.4367(4) 0.59969(13) 0.4095(3) 0.0161(7) Uani 1 1 d . . . . .
C3' C 0.3044(4) 0.58643(13) 0.3551(3) 0.0154(7) Uani 1 1 d . . . . .
C4' C 0.2636(4) 0.60743(14) 0.2675(3) 0.0167(8) Uani 1 1 d . . . . .
C5' C 0.3582(4) 0.63818(13) 0.2400(3) 0.0165(7) Uani 1 1 d . . . . .
H5' H 0.3317 0.6512 0.1811 0.020 Uiso 1 1 calc R . . . .
C6' C 0.4905(4) 0.65122(13) 0.2937(3) 0.0163(7) Uani 1 1 d . . . . .
C7' C 0.5260(4) 0.63187(14) 0.3792(3) 0.0164(7) Uani 1 1 d . . . . .
H7' H 0.6134 0.6407 0.4182 0.020 Uiso 1 1 calc R . . . .
C8' C 0.1168(4) 0.59827(14) 0.2073(3) 0.0195(8) Uani 1 1 d . . . . .
C9' C 0.0111(4) 0.61988(17) 0.2540(3) 0.0260(10) Uani 1 1 d . . . . .
H9'A H -0.0836 0.6111 0.2199 0.039 Uiso 1 1 calc GR . . . .
H9'B H 0.0205 0.6567 0.2578 0.039 Uiso 1 1 calc GR . . . .
H9'C H 0.0287 0.6057 0.3140 0.039 Uiso 1 1 calc GR . . . .
C10' C 0.0935(4) 0.54124(15) 0.1880(3) 0.0233(8) Uani 1 1 d . . . . .
H10A H 0.1126 0.5226 0.2443 0.035 Uiso 1 1 calc GR . . . .
H10B H 0.1563 0.5295 0.1530 0.035 Uiso 1 1 calc GR . . . .
H10C H -0.0033 0.5354 0.1545 0.035 Uiso 1 1 calc GR . . . .
C11' C 0.0920(4) 0.62510(15) 0.1175(3) 0.0235(8) Uani 1 1 d . . . . .
H11A H 0.1550 0.6112 0.0843 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.1100 0.6613 0.1272 0.035 Uiso 1 1 calc GR . . . .
H11C H -0.0048 0.6199 0.0833 0.035 Uiso 1 1 calc GR . . . .
C12' C 0.5860(4) 0.68509(14) 0.2557(3) 0.0181(7) Uani 1 1 d . . . . .
C13' C 0.6239(4) 0.65687(16) 0.1791(3) 0.0241(8) Uani 1 1 d . . . . .
H13A H 0.6678 0.6245 0.2008 0.036 Uiso 1 1 calc GR . . . .
H13B H 0.6889 0.6774 0.1560 0.036 Uiso 1 1 calc GR . . . .
H13C H 0.5392 0.6507 0.1315 0.036 Uiso 1 1 calc GR . . . .
C14' C 0.7212(4) 0.69839(16) 0.3259(3) 0.0257(9) Uani 1 1 d . . . . .
H14A H 0.6985 0.7155 0.3761 0.039 Uiso 1 1 calc GR . . . .
H14B H 0.7781 0.7208 0.2994 0.039 Uiso 1 1 calc GR . . . .
H14C H 0.7733 0.6674 0.3468 0.039 Uiso 1 1 calc GR . . . .
C15' C 0.5131(4) 0.73511(16) 0.2210(3) 0.0283(9) Uani 1 1 d . . . . .
H15A H 0.5757 0.7560 0.1964 0.042 Uiso 1 1 calc GR . . . .
H15B H 0.4895 0.7532 0.2700 0.042 Uiso 1 1 calc GR . . . .
H15C H 0.4278 0.7280 0.1744 0.042 Uiso 1 1 calc GR . . . .
C16' C 0.3295(4) 0.65167(13) 0.5352(3) 0.0154(7) Uani 1 1 d . . . . .
H16A H 0.2640 0.6601 0.5713 0.018 Uiso 1 1 calc R . . . .
H16B H 0.2773 0.6542 0.4718 0.018 Uiso 1 1 calc R . . . .
O3' O 0.5648(3) 0.68434(11) 0.5898(2) 0.0272(7) Uani 1 1 d . . . . .
C17' C 0.4437(4) 0.69089(14) 0.5531(3) 0.0193(8) Uani 1 1 d . . . . .
O4' O 0.3890(3) 0.73507(11) 0.5221(2) 0.0361(8) Uani 1 1 d . . . . .
C19' C 0.4836(6) 0.77823(17) 0.5332(4) 0.0449(14) Uani 1 1 d . . . . .
H19A H 0.5761 0.7675 0.5270 0.054 Uiso 1 1 calc R . . . .
H19B H 0.4956 0.7936 0.5926 0.054 Uiso 1 1 calc R . . . .
C20' C 0.4184(5) 0.81531(16) 0.4617(4) 0.0351(11) Uani 1 1 d . . . . .
H20A H 0.4155 0.8007 0.4033 0.053 Uiso 1 1 calc GR . . . .
H20B H 0.4737 0.8464 0.4699 0.053 Uiso 1 1 calc GR . . . .
H20C H 0.3234 0.8230 0.4650 0.053 Uiso 1 1 calc GR . . . .
C21' C 0.4377(4) 0.58977(15) 0.6514(3) 0.0186(8) Uani 1 1 d . . . . .
H21A H 0.4576 0.5533 0.6616 0.022 Uiso 1 1 calc R . . . .
H21B H 0.5274 0.6082 0.6700 0.022 Uiso 1 1 calc R . . . .
C22' C 0.3448(4) 0.60677(15) 0.7076(3) 0.0204(8) Uani 1 1 d . . . . .
C23' C 0.2163(4) 0.58248(16) 0.6978(3) 0.0234(8) Uani 1 1 d . . . . .
C24' C 0.1379(5) 0.5955(2) 0.7599(3) 0.0288(11) Uani 1 1 d . . . . .
C25' C 0.1871(4) 0.63391(18) 0.8209(3) 0.0293(9) Uani 1 1 d . . . . .
H25' H 0.1338 0.6422 0.8616 0.035 Uiso 1 1 calc R . . . .
C26' C 0.3091(4) 0.66100(17) 0.8266(3) 0.0255(9) Uani 1 1 d . . . . .
C27' C 0.3886(4) 0.64543(16) 0.7687(3) 0.0216(8) Uani 1 1 d . . . . .
H27' H 0.4747 0.6618 0.7714 0.026 Uiso 1 1 calc R . . . .
C28' C 0.0010(5) 0.5676(2) 0.7592(3) 0.0414(13) Uani 1 1 d . . . . .
C29' C -0.1097(5) 0.5808(2) 0.6729(4) 0.0447(13) Uani 1 1 d . . . . .
H29A H -0.1912 0.5590 0.6671 0.067 Uiso 1 1 calc GR . . . .
H29B H -0.0708 0.5757 0.6218 0.067 Uiso 1 1 calc GR . . . .
H29C H -0.1377 0.6162 0.6749 0.067 Uiso 1 1 calc GR . . . .
C30' C 0.0281(5) 0.5106(2) 0.7695(4) 0.0457(14) Uani 1 1 d . . . . .
H30A H 0.0908 0.5037 0.8282 0.069 Uiso 1 1 calc GR . . . .
H30B H 0.0712 0.4989 0.7231 0.069 Uiso 1 1 calc GR . . . .
H30C H -0.0603 0.4929 0.7638 0.069 Uiso 1 1 calc GR . . . .
C31' C -0.0605(6) 0.5844(3) 0.8364(4) 0.0608(19) Uani 1 1 d . . . . .
H31A H 0.0051 0.5759 0.8933 0.091 Uiso 1 1 calc GR . . . .
H31B H -0.1490 0.5669 0.8316 0.091 Uiso 1 1 calc GR . . . .
H31C H -0.0764 0.6210 0.8331 0.091 Uiso 1 1 calc GR . . . .
C32' C 0.3562(5) 0.70561(17) 0.8895(3) 0.0288(10) Uani 1 1 d . . . . .
C33' C 0.3355(6) 0.75472(18) 0.8343(3) 0.0380(11) Uani 1 1 d . . . . .
H33A H 0.3923 0.7535 0.7915 0.057 Uiso 1 1 calc GR . . . .
H33B H 0.3640 0.7837 0.8741 0.057 Uiso 1 1 calc GR . . . .
H33C H 0.2370 0.7582 0.8024 0.057 Uiso 1 1 calc GR . . . .
C34' C 0.5103(5) 0.70056(17) 0.9389(3) 0.0303(10) Uani 1 1 d . . . . .
H34A H 0.5256 0.6682 0.9705 0.045 Uiso 1 1 calc GR . . . .
H34B H 0.5367 0.7283 0.9817 0.045 Uiso 1 1 calc GR . . . .
H34C H 0.5672 0.7020 0.8961 0.045 Uiso 1 1 calc GR . . . .
C35' C 0.2725(6) 0.7102(2) 0.9594(3) 0.0396(12) Uani 1 1 d . . . . .
H35A H 0.1736 0.7146 0.9295 0.059 Uiso 1 1 calc GR . . . .
H35B H 0.3059 0.7394 0.9978 0.059 Uiso 1 1 calc GR . . . .
H35C H 0.2848 0.6794 0.9956 0.059 Uiso 1 1 calc GR . . . .
C36' C -0.0078(4) 0.47633(16) 0.5405(3) 0.0251(9) Uani 1 1 d . . . . .
H36A H -0.0431 0.5055 0.5681 0.030 Uiso 1 1 calc R . . . .
H36B H 0.0706 0.4614 0.5863 0.030 Uiso 1 1 calc R . . . .
C37' C -0.1236(5) 0.43702(17) 0.5151(3) 0.0311(10) Uani 1 1 d . . . . .
H37A H -0.0914 0.4083 0.4859 0.047 Uiso 1 1 calc GR . . . .
H37B H -0.2056 0.4522 0.4742 0.047 Uiso 1 1 calc GR . . . .
H37C H -0.1482 0.4253 0.5688 0.047 Uiso 1 1 calc GR . . . .
C38' C -0.0672(4) 0.51616(15) 0.3916(3) 0.0224(8) Uani 1 1 d . . . . .
H38A H -0.1330 0.4884 0.3675 0.027 Uiso 1 1 calc R . . . .
H38B H -0.0274 0.5281 0.3431 0.027 Uiso 1 1 calc R . . . .
C39' C -0.1470(4) 0.55916(16) 0.4197(3) 0.0303(10) Uani 1 1 d . . . . .
H39A H -0.0817 0.5857 0.4480 0.046 Uiso 1 1 calc GR . . . .
H39B H -0.1970 0.5466 0.4620 0.046 Uiso 1 1 calc GR . . . .
H39C H -0.2139 0.5730 0.3673 0.046 Uiso 1 1 calc GR . . . .
C40' C 0.1132(4) 0.45352(14) 0.4265(3) 0.0205(8) Uani 1 1 d . . . . .
H40A H 0.1492 0.4671 0.3775 0.025 Uiso 1 1 calc R . . . .
H40B H 0.0404 0.4283 0.4006 0.025 Uiso 1 1 calc R . . . .
C41' C 0.2310(4) 0.42715(16) 0.4927(3) 0.0235(8) Uani 1 1 d . . . . .
H41A H 0.1957 0.4124 0.5403 0.035 Uiso 1 1 calc GR . . . .
H41B H 0.3045 0.4517 0.5181 0.035 Uiso 1 1 calc GR . . . .
H41C H 0.2691 0.4003 0.4624 0.035 Uiso 1 1 calc GR . . . .
C20A C 1.0394(10) 0.7251(4) 0.6300(6) 0.038(3) Uani 0.539(12) 1 d . . P B 2
H8DA H 1.1000 0.7541 0.6520 0.057 Uiso 0.539(12) 1 calc GR . P B 2
H9DA H 1.0925 0.6938 0.6457 0.057 Uiso 0.539(12) 1 calc GR . P B 2
H0EA H 0.9607 0.7252 0.6571 0.057 Uiso 0.539(12) 1 calc GR . P B 2
C15A C 0.843(2) 0.7525(5) 0.7592(10) 0.056(5) Uani 0.402(13) 1 d D . P A 2
H1EA H 0.7598 0.7417 0.7140 0.084 Uiso 0.402(13) 1 calc GR . P A 2
H2EA H 0.8775 0.7244 0.8002 0.084 Uiso 0.402(13) 1 calc GR . P A 2
H3EA H 0.9156 0.7625 0.7302 0.084 Uiso 0.402(13) 1 calc GR . P A 2
C13A C 0.7368(6) 0.7974(2) 0.8882(4) 0.0550(16) Uani 1 1 d D . . C 2
H4EA H 0.7556 0.8293 0.9211 0.083 Uiso 1 1 calc GR . . C 2
H5EA H 0.7741 0.7692 0.9282 0.083 Uiso 1 1 calc GR . . C 2
H6EA H 0.6360 0.7931 0.8645 0.083 Uiso 1 1 calc GR . . C 2
C14A C 0.9786(15) 0.8134(6) 0.8628(10) 0.0321(18) Uani 0.402(13) 1 d D . P A 2
H7EA H 1.0297 0.8180 0.8173 0.048 Uiso 0.402(13) 1 calc GR . P A 2
H8EA H 1.0215 0.7861 0.9032 0.048 Uiso 0.402(13) 1 calc GR . P A 2
H9EA H 0.9817 0.8449 0.8966 0.048 Uiso 0.402(13) 1 calc GR . P A 2


_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 O1 2.024(4) . ?
Pd1 N2 2.133(3) . ?
Pd1 O2 2.020(4) . ?
Pd1 N1 2.082(3) . ?
O1 C3 1.339(5) . ?
N2 C36 1.496(5) . ?
N2 C38 1.502(5) . ?
N2 C40 1.506(5) . ?
C1 H 0.9900 . ?
C1 HA 0.9900 . ?
C1 N1 1.503(5) . ?
C1 C2 1.502(6) . ?
O2 C23 1.337(5) . ?
N1 C16 1.483(5) . ?
N1 C21 1.517(5) . ?
C2 C3 1.410(6) . ?
C2 C7 1.386(6) . ?
C3 C4 1.422(7) . ?
C4 C5 1.391(7) . ?
C4 C8 1.539(7) . ?
C5 HB 0.9500 . ?
C5 C6 1.400(7) . ?
C6 C7 1.395(7) . ?
C6 C12 1.524(7) . ?
C7 HC 0.9500 . ?
C8 C9 1.545(7) . ?
C8 C10 1.539(7) . ?
C8 C11 1.535(7) . ?
C9 HD 0.9800 . ?
C9 HE 0.9800 . ?
C9 HF 0.9800 . ?
C10 HG 0.9800 . ?
C10 HH 0.9800 . ?
C10 HI 0.9800 . ?
C11 HJ 0.9800 . ?
C11 HK 0.9800 . ?
C11 HL 0.9800 . ?
C12 C14 1.392(11) . ?
C12 C15 1.619(9) . ?
C12 C15A 1.556(14) . ?
C12 C13A 1.521(8) . ?
C12 C14A 1.738(15) . ?
C14 HM 0.9800 . ?
C14 HN 0.9800 . ?
C14 HO 0.9800 . ?
C15 HP 0.9800 . ?
C15 HQ 0.9800 . ?
C15 HR 0.9800 . ?
C16 HS 0.9900 . ?
C16 HT 0.9900 . ?
C16 C17 1.524(5) . ?
O3 C17 1.205(6) . ?
C17 O4 1.330(5) . ?
O4 C19 1.471(6) . ?
C19 HU 0.9900 . ?
C19 HV 0.9900 . ?
C19 HW 0.9900 . ?
C19 HX 0.9900 . ?
C19 C20 1.359(12) . ?
C19 C20A 1.420(11) . ?
C20 HY 0.9800 . ?
C20 HZ 0.9800 . ?
C20 H0AA 0.9800 . ?
C21 H1AA 0.9900 . ?
C21 H2AA 0.9900 . ?
C21 C22 1.496(6) . ?
C22 C23 1.410(5) . ?
C22 C27 1.393(5) . ?
C23 C24 1.428(6) . ?
C24 C25 1.393(6) . ?
C24 C28 1.530(5) . ?
C25 H3AA 0.9500 . ?
C25 C26 1.397(5) . ?
C26 C27 1.380(6) . ?
C26 C32 1.530(5) . ?
C27 H4AA 0.9500 . ?
C28 C29 1.543(6) . ?
C28 C30 1.543(5) . ?
C28 C31 1.538(6) . ?
C29 H5AA 0.9800 . ?
C29 H6AA 0.9800 . ?
C29 H7AA 0.9800 . ?
C30 H8AA 0.9800 . ?
C30 H9AA 0.9800 . ?
C30 H0BA 0.9800 . ?
C31 H1BA 0.9800 . ?
C31 H2BA 0.9800 . ?
C31 H3BA 0.9800 . ?
C32 C33 1.536(6) . ?
C32 C34 1.529(6) . ?
C32 C35 1.545(6) . ?
C33 H4BA 0.9800 . ?
C33 H5BA 0.9800 . ?
C33 H6BA 0.9800 . ?
C34 H7BA 0.9800 . ?
C34 H8BA 0.9800 . ?
C34 H9BA 0.9800 . ?
C35 H0CA 0.9800 . ?
C35 H1CA 0.9800 . ?
C35 H2CA 0.9800 . ?
C36 H3CA 0.9900 . ?
C36 H4CA 0.9900 . ?
C36 C37 1.520(6) . ?
C37 H5CA 0.9800 . ?
C37 H6CA 0.9800 . ?
C37 H7CA 0.9800 . ?
C38 H8CA 0.9900 . ?
C38 H9CA 0.9900 . ?
C38 C39 1.512(5) . ?
C39 H0DA 0.9800 . ?
C39 H1DA 0.9800 . ?
C39 H2DA 0.9800 . ?
C40 H3DA 0.9900 . ?
C40 H4DA 0.9900 . ?
C40 C41 1.538(6) . ?
C41 H5DA 0.9800 . ?
C41 H6DA 0.9800 . ?
C41 H7DA 0.9800 . ?
Pd1' O1' 2.031(4) . ?
Pd1' N2' 2.137(3) . ?
Pd1' O2' 2.029(4) . ?
Pd1' N1' 2.057(3) . ?
O1' C3' 1.338(5) . ?
N2' C36' 1.511(5) . ?
N2' C38' 1.495(5) . ?
N2' C40' 1.494(5) . ?
C1' H1'A 0.9900 . ?
C1' H1'B 0.9900 . ?
C1' N1' 1.509(5) . ?
C1' C2' 1.492(5) . ?
O2' C23' 1.333(6) . ?
N1' C16' 1.482(4) . ?
N1' C21' 1.502(5) . ?
C2' C3' 1.411(5) . ?
C2' C7' 1.398(5) . ?
C3' C4' 1.429(6) . ?
C4' C5' 1.393(6) . ?
C4' C8' 1.535(6) . ?
C5' H5' 0.9500 . ?
C5' C6' 1.405(5) . ?
C6' C7' 1.383(5) . ?
C6' C12' 1.532(5) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.535(5) . ?
C8' C10' 1.544(5) . ?
C8' C11' 1.530(5) . ?
C9' H9'A 0.9800 . ?
C9' H9'B 0.9800 . ?
C9' H9'C 0.9800 . ?
C10' H10A 0.9800 . ?
C10' H10B 0.9800 . ?
C10' H10C 0.9800 . ?
C11' H11A 0.9800 . ?
C11' H11B 0.9800 . ?
C11' H11C 0.9800 . ?
C12' C13' 1.535(5) . ?
C12' C14' 1.536(5) . ?
C12' C15' 1.538(5) . ?
C13' H13A 0.9800 . ?
C13' H13B 0.9800 . ?
C13' H13C 0.9800 . ?
C14' H14A 0.9800 . ?
C14' H14B 0.9800 . ?
C14' H14C 0.9800 . ?
C15' H15A 0.9800 . ?
C15' H15B 0.9800 . ?
C15' H15C 0.9800 . ?
C16' H16A 0.9900 . ?
C16' H16B 0.9900 . ?
C16' C17' 1.509(5) . ?
O3' C17' 1.203(5) . ?
C17' O4' 1.326(5) . ?
O4' C19' 1.461(5) . ?
C19' H19A 0.9900 . ?
C19' H19B 0.9900 . ?
C19' C20' 1.499(6) . ?
C20' H20A 0.9800 . ?
C20' H20B 0.9800 . ?
C20' H20C 0.9800 . ?
C21' H21A 0.9900 . ?
C21' H21B 0.9900 . ?
C21' C22' 1.497(5) . ?
C22' C23' 1.401(6) . ?
C22' C27' 1.387(6) . ?
C23' C24' 1.432(6) . ?
C24' C25' 1.392(7) . ?
C24' C28' 1.544(6) . ?
C25' H25' 0.9500 . ?
C25' C26' 1.391(6) . ?
C26' C27' 1.406(6) . ?
C26' C32' 1.527(7) . ?
C27' H27' 0.9500 . ?
C28' C29' 1.539(7) . ?
C28' C30' 1.533(8) . ?
C28' C31' 1.548(7) . ?
C29' H29A 0.9800 . ?
C29' H29B 0.9800 . ?
C29' H29C 0.9800 . ?
C30' H30A 0.9800 . ?
C30' H30B 0.9800 . ?
C30' H30C 0.9800 . ?
C31' H31A 0.9800 . ?
C31' H31B 0.9800 . ?
C31' H31C 0.9800 . ?
C32' C33' 1.542(6) . ?
C32' C34' 1.530(7) . ?
C32' C35' 1.536(6) . ?
C33' H33A 0.9800 . ?
C33' H33B 0.9800 . ?
C33' H33C 0.9800 . ?
C34' H34A 0.9800 . ?
C34' H34B 0.9800 . ?
C34' H34C 0.9800 . ?
C35' H35A 0.9800 . ?
C35' H35B 0.9800 . ?
C35' H35C 0.9800 . ?
C36' H36A 0.9900 . ?
C36' H36B 0.9900 . ?
C36' C37' 1.525(6) . ?
C37' H37A 0.9800 . ?
C37' H37B 0.9800 . ?
C37' H37C 0.9800 . ?
C38' H38A 0.9900 . ?
C38' H38B 0.9900 . ?
C38' C39' 1.515(6) . ?
C39' H39A 0.9800 . ?
C39' H39B 0.9800 . ?
C39' H39C 0.9800 . ?
C40' H40A 0.9900 . ?
C40' H40B 0.9900 . ?
C40' C41' 1.514(5) . ?
C41' H41A 0.9800 . ?
C41' H41B 0.9800 . ?
C41' H41C 0.9800 . ?
C20A H8DA 0.9800 . ?
C20A H9DA 0.9800 . ?
C20A H0EA 0.9800 . ?
C15A H1EA 0.9800 . ?
C15A H2EA 0.9800 . ?
C15A H3EA 0.9800 . ?
C13A H4EA 0.9800 . ?
C13A H5EA 0.9800 . ?
C13A H6EA 0.9800 . ?
C14A H7EA 0.9800 . ?
C14A H8EA 0.9800 . ?
C14A H9EA 0.9800 . ?

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
O1 Pd1 N2 88.64(14) . . ?
O1 Pd1 N1 93.46(14) . . ?
O2 Pd1 O1 173.79(17) . . ?
O2 Pd1 N2 86.02(13) . . ?
O2 Pd1 N1 92.35(13) . . ?
N1 Pd1 N2 169.64(12) . . ?
C3 O1 Pd1 123.0(3) . . ?
C36 N2 Pd1 106.5(2) . . ?
C36 N2 C38 106.5(3) . . ?
C36 N2 C40 109.0(3) . . ?
C38 N2 Pd1 112.2(2) . . ?
C38 N2 C40 110.7(3) . . ?
C40 N2 Pd1 111.7(3) . . ?
H C1 HA 107.9 . . ?
N1 C1 H 109.2 . . ?
N1 C1 HA 109.2 . . ?
C2 C1 H 109.2 . . ?
C2 C1 HA 109.2 . . ?
C2 C1 N1 111.8(3) . . ?
C23 O2 Pd1 124.2(3) . . ?
C1 N1 Pd1 105.9(2) . . ?
C1 N1 C21 109.5(3) . . ?
C16 N1 Pd1 113.7(2) . . ?
C16 N1 C1 111.0(3) . . ?
C16 N1 C21 112.6(3) . . ?
C21 N1 Pd1 103.6(2) . . ?
C3 C2 C1 117.9(4) . . ?
C7 C2 C1 120.9(4) . . ?
C7 C2 C3 121.2(4) . . ?
O1 C3 C2 120.5(4) . . ?
O1 C3 C4 121.5(4) . . ?
C2 C3 C4 118.0(4) . . ?
C3 C4 C8 121.9(4) . . ?
C5 C4 C3 118.1(4) . . ?
C5 C4 C8 120.0(5) . . ?
C4 C5 HB 117.9 . . ?
C4 C5 C6 124.2(5) . . ?
C6 C5 HB 117.9 . . ?
C5 C6 C12 122.2(5) . . ?
C7 C6 C5 116.2(4) . . ?
C7 C6 C12 121.6(5) . . ?
C2 C7 C6 121.8(4) . . ?
C2 C7 HC 119.1 . . ?
C6 C7 HC 119.1 . . ?
C4 C8 C9 109.7(4) . . ?
C10 C8 C4 109.3(4) . . ?
C10 C8 C9 111.1(4) . . ?
C11 C8 C4 113.2(4) . . ?
C11 C8 C9 106.6(4) . . ?
C11 C8 C10 107.1(4) . . ?
C8 C9 HD 109.5 . . ?
C8 C9 HE 109.5 . . ?
C8 C9 HF 109.5 . . ?
HD C9 HE 109.5 . . ?
HD C9 HF 109.5 . . ?
HE C9 HF 109.5 . . ?
C8 C10 HG 109.5 . . ?
C8 C10 HH 109.5 . . ?
C8 C10 HI 109.5 . . ?
HG C10 HH 109.5 . . ?
HG C10 HI 109.5 . . ?
HH C10 HI 109.5 . . ?
C8 C11 HJ 109.5 . . ?
C8 C11 HK 109.5 . . ?
C8 C11 HL 109.5 . . ?
HJ C11 HK 109.5 . . ?
HJ C11 HL 109.5 . . ?
HK C11 HL 109.5 . . ?
C6 C12 C15 106.9(4) . . ?
C6 C12 C15A 109.2(6) . . ?
C6 C12 C14A 103.2(7) . . ?
C14 C12 C6 116.8(7) . . ?
C14 C12 C15 113.3(7) . . ?
C15A C12 C14A 94.7(9) . . ?
C13A C12 C6 112.7(5) . . ?
C13A C12 C15A 128.2(8) . . ?
C13A C12 C14A 103.9(6) . . ?
C12 C14 HM 109.5 . . ?
C12 C14 HN 109.5 . . ?
C12 C14 HO 109.5 . . ?
HM C14 HN 109.5 . . ?
HM C14 HO 109.5 . . ?
HN C14 HO 109.5 . . ?
C12 C15 HP 109.5 . . ?
C12 C15 HQ 109.5 . . ?
C12 C15 HR 109.5 . . ?
HP C15 HQ 109.5 . . ?
HP C15 HR 109.5 . . ?
HQ C15 HR 109.5 . . ?
N1 C16 HS 108.6 . . ?
N1 C16 HT 108.6 . . ?
N1 C16 C17 114.9(3) . . ?
HS C16 HT 107.5 . . ?
C17 C16 HS 108.6 . . ?
C17 C16 HT 108.6 . . ?
O3 C17 C16 126.5(4) . . ?
O3 C17 O4 124.7(4) . . ?
O4 C17 C16 108.9(4) . . ?
C17 O4 C19 115.4(4) . . ?
O4 C19 HU 109.3 . . ?
O4 C19 HV 109.3 . . ?
O4 C19 HW 108.9 . . ?
O4 C19 HX 108.9 . . ?
HU C19 HV 108.0 . . ?
HW C19 HX 107.7 . . ?
C20 C19 O4 113.3(7) . . ?
C20 C19 HW 108.9 . . ?
C20 C19 HX 108.9 . . ?
C20A C19 O4 111.6(6) . . ?
C20A C19 HU 109.3 . . ?
C20A C19 HV 109.3 . . ?
C19 C20 HY 109.5 . . ?
C19 C20 HZ 109.5 . . ?
C19 C20 H0AA 109.5 . . ?
HY C20 HZ 109.5 . . ?
HY C20 H0AA 109.5 . . ?
HZ C20 H0AA 109.5 . . ?
N1 C21 H1AA 109.5 . . ?
N1 C21 H2AA 109.5 . . ?
H1AA C21 H2AA 108.0 . . ?
C22 C21 N1 110.9(3) . . ?
C22 C21 H1AA 109.5 . . ?
C22 C21 H2AA 109.5 . . ?
C23 C22 C21 118.6(3) . . ?
C27 C22 C21 120.0(3) . . ?
C27 C22 C23 121.3(4) . . ?
O2 C23 C22 121.5(4) . . ?
O2 C23 C24 120.5(4) . . ?
C22 C23 C24 118.0(3) . . ?
C23 C24 C28 121.0(3) . . ?
C25 C24 C23 118.0(4) . . ?
C25 C24 C28 121.0(4) . . ?
C24 C25 H3AA 117.9 . . ?
C24 C25 C26 124.2(4) . . ?
C26 C25 H3AA 117.9 . . ?
C25 C26 C32 119.4(4) . . ?
C27 C26 C25 116.9(3) . . ?
C27 C26 C32 123.7(3) . . ?
C22 C27 H4AA 119.2 . . ?
C26 C27 C22 121.7(4) . . ?
C26 C27 H4AA 119.2 . . ?
C24 C28 C29 109.1(3) . . ?
C24 C28 C30 109.6(3) . . ?
C24 C28 C31 113.1(3) . . ?
C29 C28 C30 110.8(3) . . ?
C31 C28 C29 106.9(3) . . ?
C31 C28 C30 107.3(3) . . ?
C28 C29 H5AA 109.5 . . ?
C28 C29 H6AA 109.5 . . ?
C28 C29 H7AA 109.5 . . ?
H5AA C29 H6AA 109.5 . . ?
H5AA C29 H7AA 109.5 . . ?
H6AA C29 H7AA 109.5 . . ?
C28 C30 H8AA 109.5 . . ?
C28 C30 H9AA 109.5 . . ?
C28 C30 H0BA 109.5 . . ?
H8AA C30 H9AA 109.5 . . ?
H8AA C30 H0BA 109.5 . . ?
H9AA C30 H0BA 109.5 . . ?
C28 C31 H1BA 109.5 . . ?
C28 C31 H2BA 109.5 . . ?
C28 C31 H3BA 109.5 . . ?
H1BA C31 H2BA 109.5 . . ?
H1BA C31 H3BA 109.5 . . ?
H2BA C31 H3BA 109.5 . . ?
C26 C32 C33 110.3(3) . . ?
C26 C32 C35 108.4(3) . . ?
C33 C32 C35 108.7(4) . . ?
C34 C32 C26 112.5(4) . . ?
C34 C32 C33 109.2(4) . . ?
C34 C32 C35 107.7(4) . . ?
C32 C33 H4BA 109.5 . . ?
C32 C33 H5BA 109.5 . . ?
C32 C33 H6BA 109.5 . . ?
H4BA C33 H5BA 109.5 . . ?
H4BA C33 H6BA 109.5 . . ?
H5BA C33 H6BA 109.5 . . ?
C32 C34 H7BA 109.5 . . ?
C32 C34 H8BA 109.5 . . ?
C32 C34 H9BA 109.5 . . ?
H7BA C34 H8BA 109.5 . . ?
H7BA C34 H9BA 109.5 . . ?
H8BA C34 H9BA 109.5 . . ?
C32 C35 H0CA 109.5 . . ?
C32 C35 H1CA 109.5 . . ?
C32 C35 H2CA 109.5 . . ?
H0CA C35 H1CA 109.5 . . ?
H0CA C35 H2CA 109.5 . . ?
H1CA C35 H2CA 109.5 . . ?
N2 C36 H3CA 108.7 . . ?
N2 C36 H4CA 108.7 . . ?
N2 C36 C37 114.0(3) . . ?
H3CA C36 H4CA 107.6 . . ?
C37 C36 H3CA 108.7 . . ?
C37 C36 H4CA 108.7 . . ?
C36 C37 H5CA 109.5 . . ?
C36 C37 H6CA 109.5 . . ?
C36 C37 H7CA 109.5 . . ?
H5CA C37 H6CA 109.5 . . ?
H5CA C37 H7CA 109.5 . . ?
H6CA C37 H7CA 109.5 . . ?
N2 C38 H8CA 108.8 . . ?
N2 C38 H9CA 108.8 . . ?
N2 C38 C39 113.6(3) . . ?
H8CA C38 H9CA 107.7 . . ?
C39 C38 H8CA 108.8 . . ?
C39 C38 H9CA 108.8 . . ?
C38 C39 H0DA 109.5 . . ?
C38 C39 H1DA 109.5 . . ?
C38 C39 H2DA 109.5 . . ?
H0DA C39 H1DA 109.5 . . ?
H0DA C39 H2DA 109.5 . . ?
H1DA C39 H2DA 109.5 . . ?
N2 C40 H3DA 108.2 . . ?
N2 C40 H4DA 108.2 . . ?
N2 C40 C41 116.4(4) . . ?
H3DA C40 H4DA 107.3 . . ?
C41 C40 H3DA 108.2 . . ?
C41 C40 H4DA 108.2 . . ?
C40 C41 H5DA 109.5 . . ?
C40 C41 H6DA 109.5 . . ?
C40 C41 H7DA 109.5 . . ?
H5DA C41 H6DA 109.5 . . ?
H5DA C41 H7DA 109.5 . . ?
H6DA C41 H7DA 109.5 . . ?
O1' Pd1' N2' 86.08(13) . . ?
O1' Pd1' N1' 91.26(13) . . ?
O2' Pd1' O1' 174.53(17) . . ?
O2' Pd1' N2' 90.04(14) . . ?
O2' Pd1' N1' 93.05(14) . . ?
N1' Pd1' N2' 172.61(13) . . ?
C3' O1' Pd1' 124.9(3) . . ?
C36' N2' Pd1' 110.8(2) . . ?
C38' N2' Pd1' 111.0(2) . . ?
C38' N2' C36' 110.8(3) . . ?
C40' N2' Pd1' 107.4(2) . . ?
C40' N2' C36' 110.1(3) . . ?
C40' N2' C38' 106.6(3) . . ?
H1'A C1' H1'B 108.0 . . ?
N1' C1' H1'A 109.3 . . ?
N1' C1' H1'B 109.3 . . ?
C2' C1' H1'A 109.3 . . ?
C2' C1' H1'B 109.3 . . ?
C2' C1' N1' 111.4(3) . . ?
C23' O2' Pd1' 123.6(3) . . ?
C1' N1' Pd1' 105.5(2) . . ?
C16' N1' Pd1' 109.2(2) . . ?
C16' N1' C1' 112.9(3) . . ?
C16' N1' C21' 111.8(3) . . ?
C21' N1' Pd1' 108.6(2) . . ?
C21' N1' C1' 108.5(3) . . ?
C3' C2' C1' 119.1(3) . . ?
C7' C2' C1' 119.3(3) . . ?
C7' C2' C3' 121.5(3) . . ?
O1' C3' C2' 121.4(4) . . ?
O1' C3' C4' 120.9(4) . . ?
C2' C3' C4' 117.8(3) . . ?
C3' C4' C8' 120.7(3) . . ?
C5' C4' C3' 118.3(4) . . ?
C5' C4' C8' 121.0(4) . . ?
C4' C5' H5' 117.9 . . ?
C4' C5' C6' 124.2(4) . . ?
C6' C5' H5' 117.9 . . ?
C5' C6' C12' 119.4(3) . . ?
C7' C6' C5' 116.6(3) . . ?
C7' C6' C12' 124.0(3) . . ?
C2' C7' H7' 119.2 . . ?
C6' C7' C2' 121.6(3) . . ?
C6' C7' H7' 119.2 . . ?
C4' C8' C9' 108.1(3) . . ?
C4' C8' C10' 110.1(3) . . ?
C9' C8' C10' 111.7(3) . . ?
C11' C8' C4' 112.8(3) . . ?
C11' C8' C9' 107.0(3) . . ?
C11' C8' C10' 107.2(3) . . ?
C8' C9' H9'A 109.5 . . ?
C8' C9' H9'B 109.5 . . ?
C8' C9' H9'C 109.5 . . ?
H9'A C9' H9'B 109.5 . . ?
H9'A C9' H9'C 109.5 . . ?
H9'B C9' H9'C 109.5 . . ?
C8' C10' H10A 109.5 . . ?
C8' C10' H10B 109.5 . . ?
C8' C10' H10C 109.5 . . ?
H10A C10' H10B 109.5 . . ?
H10A C10' H10C 109.5 . . ?
H10B C10' H10C 109.5 . . ?
C8' C11' H11A 109.5 . . ?
C8' C11' H11B 109.5 . . ?
C8' C11' H11C 109.5 . . ?
H11A C11' H11B 109.5 . . ?
H11A C11' H11C 109.5 . . ?
H11B C11' H11C 109.5 . . ?
C6' C12' C13' 108.5(3) . . ?
C6' C12' C14' 112.0(3) . . ?
C6' C12' C15' 110.9(3) . . ?
C13' C12' C14' 108.6(3) . . ?
C13' C12' C15' 109.5(3) . . ?
C14' C12' C15' 107.3(3) . . ?
C12' C13' H13A 109.5 . . ?
C12' C13' H13B 109.5 . . ?
C12' C13' H13C 109.5 . . ?
H13A C13' H13B 109.5 . . ?
H13A C13' H13C 109.5 . . ?
H13B C13' H13C 109.5 . . ?
C12' C14' H14A 109.5 . . ?
C12' C14' H14B 109.5 . . ?
C12' C14' H14C 109.5 . . ?
H14A C14' H14B 109.5 . . ?
H14A C14' H14C 109.5 . . ?
H14B C14' H14C 109.5 . . ?
C12' C15' H15A 109.5 . . ?
C12' C15' H15B 109.5 . . ?
C12' C15' H15C 109.5 . . ?
H15A C15' H15B 109.5 . . ?
H15A C15' H15C 109.5 . . ?
H15B C15' H15C 109.5 . . ?
N1' C16' H16A 108.2 . . ?
N1' C16' H16B 108.2 . . ?
N1' C16' C17' 116.2(3) . . ?
H16A C16' H16B 107.4 . . ?
C17' C16' H16A 108.2 . . ?
C17' C16' H16B 108.2 . . ?
O3' C17' C16' 126.8(3) . . ?
O3' C17' O4' 124.4(4) . . ?
O4' C17' C16' 108.8(3) . . ?
C17' O4' C19' 117.1(3) . . ?
O4' C19' H19A 110.4 . . ?
O4' C19' H19B 110.4 . . ?
O4' C19' C20' 106.5(4) . . ?
H19A C19' H19B 108.6 . . ?
C20' C19' H19A 110.4 . . ?
C20' C19' H19B 110.4 . . ?
C19' C20' H20A 109.5 . . ?
C19' C20' H20B 109.5 . . ?
C19' C20' H20C 109.5 . . ?
H20A C20' H20B 109.5 . . ?
H20A C20' H20C 109.5 . . ?
H20B C20' H20C 109.5 . . ?
N1' C21' H21A 109.0 . . ?
N1' C21' H21B 109.0 . . ?
H21A C21' H21B 107.8 . . ?
C22' C21' N1' 112.7(3) . . ?
C22' C21' H21A 109.0 . . ?
C22' C21' H21B 109.0 . . ?
C23' C22' C21' 118.7(4) . . ?
C27' C22' C21' 119.4(3) . . ?
C27' C22' C23' 121.9(4) . . ?
O2' C23' C22' 121.2(4) . . ?
O2' C23' C24' 121.7(4) . . ?
C22' C23' C24' 117.1(4) . . ?
C23' C24' C28' 120.9(5) . . ?
C25' C24' C23' 118.7(4) . . ?
C25' C24' C28' 120.4(4) . . ?
C24' C25' H25' 117.8 . . ?
C26' C25' C24' 124.5(4) . . ?
C26' C25' H25' 117.8 . . ?
C25' C26' C27' 115.7(4) . . ?
C25' C26' C32' 123.8(4) . . ?
C27' C26' C32' 120.5(4) . . ?
C22' C27' C26' 121.8(4) . . ?
C22' C27' H27' 119.1 . . ?
C26' C27' H27' 119.1 . . ?
C24' C28' C31' 112.5(5) . . ?
C29' C28' C24' 109.1(4) . . ?
C29' C28' C31' 106.0(4) . . ?
C30' C28' C24' 109.8(4) . . ?
C30' C28' C29' 112.4(5) . . ?
C30' C28' C31' 107.1(5) . . ?
C28' C29' H29A 109.5 . . ?
C28' C29' H29B 109.5 . . ?
C28' C29' H29C 109.5 . . ?
H29A C29' H29B 109.5 . . ?
H29A C29' H29C 109.5 . . ?
H29B C29' H29C 109.5 . . ?
C28' C30' H30A 109.5 . . ?
C28' C30' H30B 109.5 . . ?
C28' C30' H30C 109.5 . . ?
H30A C30' H30B 109.5 . . ?
H30A C30' H30C 109.5 . . ?
H30B C30' H30C 109.5 . . ?
C28' C31' H31A 109.5 . . ?
C28' C31' H31B 109.5 . . ?
C28' C31' H31C 109.5 . . ?
H31A C31' H31B 109.5 . . ?
H31A C31' H31C 109.5 . . ?
H31B C31' H31C 109.5 . . ?
C26' C32' C33' 108.7(4) . . ?
C26' C32' C34' 110.8(4) . . ?
C26' C32' C35' 112.5(4) . . ?
C34' C32' C33' 109.0(4) . . ?
C34' C32' C35' 107.8(4) . . ?
C35' C32' C33' 108.1(4) . . ?
C32' C33' H33A 109.5 . . ?
C32' C33' H33B 109.5 . . ?
C32' C33' H33C 109.5 . . ?
H33A C33' H33B 109.5 . . ?
H33A C33' H33C 109.5 . . ?
H33B C33' H33C 109.5 . . ?
C32' C34' H34A 109.5 . . ?
C32' C34' H34B 109.5 . . ?
C32' C34' H34C 109.5 . . ?
H34A C34' H34B 109.5 . . ?
H34A C34' H34C 109.5 . . ?
H34B C34' H34C 109.5 . . ?
C32' C35' H35A 109.5 . . ?
C32' C35' H35B 109.5 . . ?
C32' C35' H35C 109.5 . . ?
H35A C35' H35B 109.5 . . ?
H35A C35' H35C 109.5 . . ?
H35B C35' H35C 109.5 . . ?
N2' C36' H36A 108.3 . . ?
N2' C36' H36B 108.3 . . ?
N2' C36' C37' 115.8(4) . . ?
H36A C36' H36B 107.4 . . ?
C37' C36' H36A 108.3 . . ?
C37' C36' H36B 108.3 . . ?
C36' C37' H37A 109.5 . . ?
C36' C37' H37B 109.5 . . ?
C36' C37' H37C 109.5 . . ?
H37A C37' H37B 109.5 . . ?
H37A C37' H37C 109.5 . . ?
H37B C37' H37C 109.5 . . ?
N2' C38' H38A 108.8 . . ?
N2' C38' H38B 108.8 . . ?
N2' C38' C39' 113.9(4) . . ?
H38A C38' H38B 107.7 . . ?
C39' C38' H38A 108.8 . . ?
C39' C38' H38B 108.8 . . ?
C38' C39' H39A 109.5 . . ?
C38' C39' H39B 109.5 . . ?
C38' C39' H39C 109.5 . . ?
H39A C39' H39B 109.5 . . ?
H39A C39' H39C 109.5 . . ?
H39B C39' H39C 109.5 . . ?
N2' C40' H40A 108.7 . . ?
N2' C40' H40B 108.7 . . ?
N2' C40' C41' 114.1(3) . . ?
H40A C40' H40B 107.6 . . ?
C41' C40' H40A 108.7 . . ?
C41' C40' H40B 108.7 . . ?
C40' C41' H41A 109.5 . . ?
C40' C41' H41B 109.5 . . ?
C40' C41' H41C 109.5 . . ?
H41A C41' H41B 109.5 . . ?
H41A C41' H41C 109.5 . . ?
H41B C41' H41C 109.5 . . ?
C19 C20A H8DA 109.5 . . ?
C19 C20A H9DA 109.5 . . ?
C19 C20A H0EA 109.5 . . ?
H8DA C20A H9DA 109.5 . . ?
H8DA C20A H0EA 109.5 . . ?
H9DA C20A H0EA 109.5 . . ?
C12 C15A H1EA 109.5 . . ?
C12 C15A H2EA 109.5 . . ?
C12 C15A H3EA 109.5 . . ?
H1EA C15A H2EA 109.5 . . ?
H1EA C15A H3EA 109.5 . . ?
H2EA C15A H3EA 109.5 . . ?
C12 C13A H4EA 109.5 . . ?
C12 C13A H5EA 109.5 . . ?
C12 C13A H6EA 109.5 . . ?
H4EA C13A H5EA 109.5 . . ?
H4EA C13A H6EA 109.5 . . ?
H5EA C13A H6EA 109.5 . . ?
C12 C14A H7EA 109.5 . . ?
C12 C14A H8EA 109.5 . . ?
C12 C14A H9EA 109.5 . . ?
H7EA C14A H8EA 109.5 . . ?
H7EA C14A H9EA 109.5 . . ?
H8EA C14A H9EA 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 O1 C3 C2 37.9(5) . . . . ?
Pd1 O1 C3 C4 -143.8(3) . . . . ?
Pd1 N2 C36 C37 -61.8(4) . . . . ?
Pd1 N2 C38 C39 65.2(4) . . . . ?
Pd1 N2 C40 C41 179.9(3) . . . . ?
Pd1 O2 C23 C22 -34.6(5) . . . . ?
Pd1 O2 C23 C24 145.7(3) . . . . ?
Pd1 N1 C16 C17 -179.5(3) . . . . ?
Pd1 N1 C21 C22 -76.9(3) . . . . ?
O1 C3 C4 C5 175.2(4) . . . . ?
O1 C3 C4 C8 -6.0(6) . . . . ?
C1 N1 C16 C17 -60.1(4) . . . . ?
C1 N1 C21 C22 170.5(3) . . . . ?
C1 C2 C3 O1 5.2(6) . . . . ?
C1 C2 C3 C4 -173.2(4) . . . . ?
C1 C2 C7 C6 177.8(4) . . . . ?
O2 C23 C24 C25 179.0(4) . . . . ?
O2 C23 C24 C28 -2.0(6) . . . . ?
N1 C1 C2 C3 -67.7(4) . . . . ?
N1 C1 C2 C7 112.0(4) . . . . ?
N1 C16 C17 O3 -15.8(6) . . . . ?
N1 C16 C17 O4 163.2(4) . . . . ?
N1 C21 C22 C23 60.6(5) . . . . ?
N1 C21 C22 C27 -116.2(4) . . . . ?
C2 C1 N1 Pd1 71.0(3) . . . . ?
C2 C1 N1 C16 -52.9(4) . . . . ?
C2 C1 N1 C21 -177.8(3) . . . . ?
C2 C3 C4 C5 -6.4(6) . . . . ?
C2 C3 C4 C8 172.4(4) . . . . ?
C3 C2 C7 C6 -2.5(6) . . . . ?
C3 C4 C5 C6 1.6(7) . . . . ?
C3 C4 C8 C9 66.7(6) . . . . ?
C3 C4 C8 C10 -55.3(6) . . . . ?
C3 C4 C8 C11 -174.5(5) . . . . ?
C4 C5 C6 C7 2.9(7) . . . . ?
C4 C5 C6 C12 -174.8(4) . . . . ?
C5 C4 C8 C9 -114.4(5) . . . . ?
C5 C4 C8 C10 123.6(5) . . . . ?
C5 C4 C8 C11 4.4(7) . . . . ?
C5 C6 C7 C2 -2.4(6) . . . . ?
C5 C6 C12 C14 -149.4(7) . . . . ?
C5 C6 C12 C15 82.5(6) . . . . ?
C5 C6 C12 C15A 126.4(9) . . . . ?
C5 C6 C12 C13A -22.4(7) . . . . ?
C5 C6 C12 C14A -133.8(7) . . . . ?
C7 C2 C3 O1 -174.6(4) . . . . ?
C7 C2 C3 C4 7.0(6) . . . . ?
C7 C6 C12 C14 33.1(8) . . . . ?
C7 C6 C12 C15 -95.0(6) . . . . ?
C7 C6 C12 C15A -51.2(10) . . . . ?
C7 C6 C12 C13A 160.1(5) . . . . ?
C7 C6 C12 C14A 48.7(7) . . . . ?
C8 C4 C5 C6 -177.3(4) . . . . ?
C12 C6 C7 C2 175.2(4) . . . . ?
C16 N1 C21 C22 46.5(4) . . . . ?
C16 C17 O4 C19 176.0(4) . . . . ?
O3 C17 O4 C19 -4.9(7) . . . . ?
C17 O4 C19 C20 165.5(7) . . . . ?
C17 O4 C19 C20A 89.8(7) . . . . ?
C21 N1 C16 C17 63.0(4) . . . . ?
C21 C22 C23 O2 2.7(6) . . . . ?
C21 C22 C23 C24 -177.5(3) . . . . ?
C21 C22 C27 C26 178.1(4) . . . . ?
C22 C23 C24 C25 -0.7(5) . . . . ?
C22 C23 C24 C28 178.3(3) . . . . ?
C23 C22 C27 C26 1.3(6) . . . . ?
C23 C24 C25 C26 1.7(6) . . . . ?
C23 C24 C28 C29 -59.9(5) . . . . ?
C23 C24 C28 C30 61.6(5) . . . . ?
C23 C24 C28 C31 -178.7(4) . . . . ?
C24 C25 C26 C27 -1.1(6) . . . . ?
C24 C25 C26 C32 -179.4(4) . . . . ?
C25 C24 C28 C29 119.1(4) . . . . ?
C25 C24 C28 C30 -119.4(4) . . . . ?
C25 C24 C28 C31 0.3(5) . . . . ?
C25 C26 C27 C22 -0.4(6) . . . . ?
C25 C26 C32 C33 -51.8(5) . . . . ?
C25 C26 C32 C34 -174.0(4) . . . . ?
C25 C26 C32 C35 67.1(5) . . . . ?
C27 C22 C23 O2 179.6(4) . . . . ?
C27 C22 C23 C24 -0.7(6) . . . . ?
C27 C26 C32 C33 130.0(4) . . . . ?
C27 C26 C32 C34 7.8(6) . . . . ?
C27 C26 C32 C35 -111.1(4) . . . . ?
C28 C24 C25 C26 -177.4(4) . . . . ?
C32 C26 C27 C22 177.8(4) . . . . ?
C36 N2 C38 C39 -178.6(3) . . . . ?
C36 N2 C40 C41 62.5(5) . . . . ?
C38 N2 C36 C37 178.3(3) . . . . ?
C38 N2 C40 C41 -54.3(5) . . . . ?
C40 N2 C36 C37 58.8(4) . . . . ?
C40 N2 C38 C39 -60.2(4) . . . . ?
Pd1' O1' C3' C2' 33.3(5) . . . . ?
Pd1' O1' C3' C4' -146.2(3) . . . . ?
Pd1' N2' C36' C37' 178.6(3) . . . . ?
Pd1' N2' C38' C39' -64.3(4) . . . . ?
Pd1' N2' C40' C41' 62.4(3) . . . . ?
Pd1' O2' C23' C22' -36.3(5) . . . . ?
Pd1' O2' C23' C24' 145.8(4) . . . . ?
Pd1' N1' C16' C17' -173.9(3) . . . . ?
Pd1' N1' C21' C22' -67.5(3) . . . . ?
O1' C3' C4' C5' -178.2(3) . . . . ?
O1' C3' C4' C8' 4.6(5) . . . . ?
C1' N1' C16' C17' -56.8(4) . . . . ?
C1' N1' C21' C22' 178.2(3) . . . . ?
C1' C2' C3' O1' -4.4(5) . . . . ?
C1' C2' C3' C4' 175.2(3) . . . . ?
C1' C2' C7' C6' -177.3(3) . . . . ?
O2' C23' C24' C25' -176.8(4) . . . . ?
O2' C23' C24' C28' 3.0(7) . . . . ?
N1' C1' C2' C3' -56.8(4) . . . . ?
N1' C1' C2' C7' 119.0(4) . . . . ?
N1' C16' C17' O3' -8.8(6) . . . . ?
N1' C16' C17' O4' 171.7(3) . . . . ?
N1' C21' C22' C23' 64.0(4) . . . . ?
N1' C21' C22' C27' -116.9(4) . . . . ?
C2' C1' N1' Pd1' 76.4(3) . . . . ?
C2' C1' N1' C16' -42.8(4) . . . . ?
C2' C1' N1' C21' -167.3(3) . . . . ?
C2' C3' C4' C5' 2.3(5) . . . . ?
C2' C3' C4' C8' -174.9(3) . . . . ?
C3' C2' C7' C6' -1.6(5) . . . . ?
C3' C4' C5' C6' -1.9(6) . . . . ?
C3' C4' C8' C9' 60.3(4) . . . . ?
C3' C4' C8' C10' -62.0(5) . . . . ?
C3' C4' C8' C11' 178.3(3) . . . . ?
C4' C5' C6' C7' -0.2(5) . . . . ?
C4' C5' C6' C12' 179.6(3) . . . . ?
C5' C4' C8' C9' -116.9(4) . . . . ?
C5' C4' C8' C10' 120.9(4) . . . . ?
C5' C4' C8' C11' 1.2(5) . . . . ?
C5' C6' C7' C2' 2.0(5) . . . . ?
C5' C6' C12' C13' -64.3(4) . . . . ?
C5' C6' C12' C14' 175.8(3) . . . . ?
C5' C6' C12' C15' 55.9(5) . . . . ?
C7' C2' C3' O1' 179.8(3) . . . . ?
C7' C2' C3' C4' -0.6(5) . . . . ?
C7' C6' C12' C13' 115.4(4) . . . . ?
C7' C6' C12' C14' -4.4(5) . . . . ?
C7' C6' C12' C15' -124.3(4) . . . . ?
C8' C4' C5' C6' 175.2(3) . . . . ?
C12' C6' C7' C2' -177.8(3) . . . . ?
C16' N1' C21' C22' 53.1(4) . . . . ?
C16' C17' O4' C19' 180.0(4) . . . . ?
O3' C17' O4' C19' 0.5(7) . . . . ?
C17' O4' C19' C20' 155.3(4) . . . . ?
C21' N1' C16' C17' 65.9(4) . . . . ?
C21' C22' C23' O2' -5.4(6) . . . . ?
C21' C22' C23' C24' 172.7(4) . . . . ?
C21' C22' C27' C26' -176.4(4) . . . . ?
C22' C23' C24' C25' 5.2(6) . . . . ?
C22' C23' C24' C28' -175.0(4) . . . . ?
C23' C22' C27' C26' 2.7(6) . . . . ?
C23' C24' C25' C26' -0.3(7) . . . . ?
C23' C24' C28' C29' -67.5(6) . . . . ?
C23' C24' C28' C30' 56.1(6) . . . . ?
C23' C24' C28' C31' 175.3(5) . . . . ?
C24' C25' C26' C27' -3.5(6) . . . . ?
C24' C25' C26' C32' 175.4(4) . . . . ?
C25' C24' C28' C29' 112.4(5) . . . . ?
C25' C24' C28' C30' -124.1(5) . . . . ?
C25' C24' C28' C31' -4.9(7) . . . . ?
C25' C26' C27' C22' 2.4(6) . . . . ?
C25' C26' C32' C33' -107.2(5) . . . . ?
C25' C26' C32' C34' 133.1(4) . . . . ?
C25' C26' C32' C35' 12.4(6) . . . . ?
C27' C22' C23' O2' 175.5(4) . . . . ?
C27' C22' C23' C24' -6.4(6) . . . . ?
C27' C26' C32' C33' 71.7(5) . . . . ?
C27' C26' C32' C34' -48.0(5) . . . . ?
C27' C26' C32' C35' -168.7(4) . . . . ?
C28' C24' C25' C26' 179.9(4) . . . . ?
C32' C26' C27' C22' -176.6(4) . . . . ?
C36' N2' C38' C39' 59.2(4) . . . . ?
C36' N2' C40' C41' -58.3(4) . . . . ?
C38' N2' C36' C37' 55.0(5) . . . . ?
C38' N2' C40' C41' -178.6(3) . . . . ?
C40' N2' C36' C37' -62.7(4) . . . . ?
C40' N2' C38' C39' 179.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_cu_8v00516_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2070846'
loop_
_audit_author_name
_audit_author_address
'Georgina Rosair'
;Heriot Watt University
United Kingdom
;
_audit_update_record             
;
2021-11-03 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT215_cu_8v00516_0ma_a    
;
PROBLEM: Disordered C4        has ADP max/min Ratio .....        3.8 Note
RESPONSE: disordered ethyl group modelled as two conformations  
;
# Added during the CSD deposition process: Wednesday 03 November 2021 03:11 PM
# end Validation Reply Form

_audit_creation_date             2021-10-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H53 N O4'
_chemical_formula_sum            'C34.50 H54 Cl N O4'
_chemical_formula_weight         582.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.4965(2)
_cell_length_b                   19.9546(3)
_cell_length_c                   12.0794(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.8657(8)
_cell_angle_gamma                90
_cell_volume                     3392.41(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      70.136
_cell_measurement_theta_min      3.844
_shelx_estimated_absorpt_T_max   0.928
_shelx_estimated_absorpt_T_min   0.718
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1142 before and 0.0573 after correction.
The Ratio of minimum to maximum transmission is 0.8740.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46320
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.179
_diffrn_reflns_theta_min         3.140
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5659
_reflns_number_total             6446
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6446
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0415
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0442P)²+1.3439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1065
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(C27A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2)
 Fixed Sof: H3AA(0.5) H3AB(0.5) H3BC(0.5) H3BD(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 H4C(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3AA,H3AB), C3(H3BC,H3BD), C5(H5A,H5B), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C24(H24), C26(H26)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C17A(H17D,H17E,
 H17F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C28A(H28D,H28E,H28F),
 C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.52812(6) 0.36565(4) 0.31199(8) 0.02444(19) Uani 1 1 d . . . . .
H1 H 0.573628 0.364353 0.370019 0.037 Uiso 1 1 calc R U . . .
O2 O 0.71357(7) 0.36422(5) 0.22463(9) 0.0312(2) Uani 1 1 d . . . . .
H2 H 0.691480 0.347896 0.276982 0.047 Uiso 1 1 calc R U . . .
O3 O 0.67360(7) 0.40880(5) 0.49694(8) 0.0343(2) Uani 1 1 d . . . . .
O4 O 0.80264(9) 0.40081(7) 0.64090(10) 0.0613(4) Uani 1 1 d . . . . .
N1 N 0.71069(7) 0.28718(5) 0.40894(8) 0.0219(2) Uani 1 1 d . . . . .
C1 C 0.77850(9) 0.31388(7) 0.50830(11) 0.0274(3) Uani 1 1 d . . . . .
H1A H 0.840541 0.321017 0.489358 0.033 Uiso 1 1 calc R U . . .
H1B H 0.787810 0.281044 0.571452 0.033 Uiso 1 1 calc R U . . .
C2 C 0.74387(9) 0.37918(7) 0.54610(11) 0.0297(3) Uani 1 1 d . . . . .
C3 C 0.77968(17) 0.46590(12) 0.68449(19) 0.0809(9) Uani 1 1 d . . . . .
H3AA H 0.710932 0.475156 0.656493 0.097 Uiso 0.5 1 calc R U P A 1
H3AB H 0.794901 0.464964 0.768865 0.097 Uiso 0.5 1 calc R U P A 1
H3BC H 0.732876 0.459468 0.731281 0.097 Uiso 0.5 1 calc R U P B 2
H3BD H 0.750841 0.495585 0.619771 0.097 Uiso 0.5 1 calc R U P B 2
C4 C 0.8308(4) 0.5148(2) 0.6486(7) 0.119(3) Uani 0.5 1 d . . P C 1
H4A H 0.898254 0.502681 0.668451 0.178 Uiso 0.5 1 calc R U P C 1
H4B H 0.821934 0.557202 0.685657 0.178 Uiso 0.5 1 calc R U P C 1
H4C H 0.809032 0.519825 0.565698 0.178 Uiso 0.5 1 calc R U P C 1
C4A C 0.8663(3) 0.4976(3) 0.7542(5) 0.0807(16) Uani 0.5 1 d . . P C 2
H4AA H 0.897635 0.466559 0.814470 0.121 Uiso 0.5 1 calc R U P C 2
H4AB H 0.849059 0.538722 0.788764 0.121 Uiso 0.5 1 calc R U P C 2
H4AC H 0.909610 0.508452 0.705807 0.121 Uiso 0.5 1 calc R U P C 2
C5 C 0.62749(9) 0.25550(6) 0.43974(11) 0.0239(3) Uani 1 1 d . . . . .
H5A H 0.605377 0.284276 0.494980 0.029 Uiso 1 1 calc R U . . .
H5B H 0.646284 0.211585 0.476363 0.029 Uiso 1 1 calc R U . . .
C6 C 0.54811(8) 0.24584(6) 0.33493(10) 0.0219(2) Uani 1 1 d . . . . .
C7 C 0.50406(8) 0.30169(6) 0.27456(10) 0.0213(2) Uani 1 1 d . . . . .
C8 C 0.43399(8) 0.29392(6) 0.17250(11) 0.0232(3) Uani 1 1 d . . . . .
C9 C 0.40932(9) 0.22861(6) 0.13637(11) 0.0255(3) Uani 1 1 d . . . . .
H9 H 0.361873 0.222562 0.067687 0.031 Uiso 1 1 calc R U . . .
C10 C 0.45027(9) 0.17137(6) 0.19525(11) 0.0246(3) Uani 1 1 d . . . . .
C11 C 0.52042(9) 0.18167(6) 0.29437(11) 0.0238(3) Uani 1 1 d . . . . .
H11 H 0.550442 0.143935 0.335794 0.029 Uiso 1 1 calc R U . . .
C12 C 0.38698(9) 0.35516(6) 0.10406(11) 0.0270(3) Uani 1 1 d . . . . .
C13 C 0.33489(10) 0.39668(7) 0.17780(13) 0.0342(3) Uani 1 1 d . . . . .
H13A H 0.287916 0.368426 0.201804 0.051 Uiso 1 1 calc R U . . .
H13B H 0.302671 0.434626 0.133265 0.051 Uiso 1 1 calc R U . . .
H13C H 0.380951 0.413415 0.245254 0.051 Uiso 1 1 calc R U . . .
C14 C 0.31457(11) 0.33432(8) -0.00484(14) 0.0428(4) Uani 1 1 d . . . . .
H14A H 0.346334 0.307557 -0.052774 0.064 Uiso 1 1 calc R U . . .
H14B H 0.286834 0.374439 -0.046669 0.064 Uiso 1 1 calc R U . . .
H14C H 0.264197 0.307637 0.015220 0.064 Uiso 1 1 calc R U . . .
C15 C 0.46227(10) 0.39849(7) 0.06724(11) 0.0288(3) Uani 1 1 d . . . . .
H15A H 0.509295 0.413802 0.134984 0.043 Uiso 1 1 calc R U . . .
H15B H 0.431460 0.437375 0.024217 0.043 Uiso 1 1 calc R U . . .
H15C H 0.493991 0.371873 0.019063 0.043 Uiso 1 1 calc R U . . .
C16 C 0.41679(10) 0.10127(6) 0.15045(12) 0.0289(3) Uani 1 1 d . . . . .
C17 C 0.30764(18) 0.09505(11) 0.1422(3) 0.0434(7) Uani 0.804(6) 1 d . . P D 1
H17A H 0.286094 0.049873 0.116483 0.065 Uiso 0.804(6) 1 calc R U P D 1
H17B H 0.273210 0.128092 0.087669 0.065 Uiso 0.804(6) 1 calc R U P D 1
H17C H 0.295330 0.103298 0.217360 0.065 Uiso 0.804(6) 1 calc R U P D 1
C18 C 0.43220(19) 0.09101(13) 0.0320(2) 0.0342(6) Uani 0.804(6) 1 d . . P D 1
H18A H 0.407860 0.046910 0.003291 0.051 Uiso 0.804(6) 1 calc R U P D 1
H18B H 0.500269 0.093540 0.034976 0.051 Uiso 0.804(6) 1 calc R U P D 1
H18C H 0.398444 0.125948 -0.019021 0.051 Uiso 0.804(6) 1 calc R U P D 1
C19 C 0.4656(2) 0.04550(9) 0.22779(19) 0.0450(7) Uani 0.804(6) 1 d . . P D 1
H19A H 0.452168 0.050288 0.303125 0.067 Uiso 0.804(6) 1 calc R U P D 1
H19B H 0.534368 0.048058 0.235300 0.067 Uiso 0.804(6) 1 calc R U P D 1
H19C H 0.441950 0.002081 0.194980 0.067 Uiso 0.804(6) 1 calc R U P D 1
C20 C 0.75752(9) 0.24030(6) 0.34490(11) 0.0233(3) Uani 1 1 d . . . . .
H20A H 0.708278 0.216615 0.287210 0.028 Uiso 1 1 calc R U . . .
H20B H 0.793096 0.206334 0.398140 0.028 Uiso 1 1 calc R U . . .
C21 C 0.82495(8) 0.27511(6) 0.28586(10) 0.0218(2) Uani 1 1 d . . . . .
C22 C 0.79873(9) 0.33477(6) 0.22568(11) 0.0240(3) Uani 1 1 d . . . . .
C23 C 0.85855(10) 0.36518(6) 0.16429(13) 0.0302(3) Uani 1 1 d . . . . .
C24 C 0.94370(10) 0.33236(7) 0.16531(12) 0.0307(3) Uani 1 1 d . . . . .
H24 H 0.984858 0.351867 0.123789 0.037 Uiso 1 1 calc R U . . .
C25 C 0.97226(9) 0.27232(7) 0.22389(11) 0.0267(3) Uani 1 1 d . . . . .
C26 C 0.91163(9) 0.24519(6) 0.28521(10) 0.0239(3) Uani 1 1 d . . . . .
H26 H 0.929667 0.205266 0.327739 0.029 Uiso 1 1 calc R U . . .
C27 C 0.8261(4) 0.4327(2) 0.0928(5) 0.0207(9) Uani 0.652(14) 1 d . . P E 1
C28 C 0.8222(4) 0.4871(2) 0.1809(4) 0.0382(9) Uani 0.652(14) 1 d . . P E 1
H28A H 0.803829 0.529825 0.141882 0.057 Uiso 0.652(14) 1 calc R U P E 1
H28B H 0.884843 0.491674 0.233521 0.057 Uiso 0.652(14) 1 calc R U P E 1
H28C H 0.775331 0.474594 0.223826 0.057 Uiso 0.652(14) 1 calc R U P E 1
C29 C 0.7291(4) 0.4271(3) 0.0072(5) 0.0255(8) Uani 0.652(14) 1 d . . P E 1
H29A H 0.711644 0.470774 -0.029075 0.038 Uiso 0.652(14) 1 calc R U P E 1
H29B H 0.680923 0.413290 0.047257 0.038 Uiso 0.652(14) 1 calc R U P E 1
H29C H 0.732817 0.393857 -0.051246 0.038 Uiso 0.652(14) 1 calc R U P E 1
C30 C 0.8990(3) 0.45290(15) 0.0257(5) 0.0326(9) Uani 0.652(14) 1 d . . P E 1
H30A H 0.902234 0.418089 -0.030498 0.049 Uiso 0.652(14) 1 calc R U P E 1
H30B H 0.961535 0.458124 0.078232 0.049 Uiso 0.652(14) 1 calc R U P E 1
H30C H 0.879776 0.495435 -0.013682 0.049 Uiso 0.652(14) 1 calc R U P E 1
C31 C 1.06796(10) 0.24024(8) 0.22144(12) 0.0348(3) Uani 1 1 d . . . . .
C32 C 1.14809(10) 0.28347(9) 0.29291(17) 0.0496(4) Uani 1 1 d . . . . .
H32A H 1.143174 0.329148 0.262246 0.074 Uiso 1 1 calc R U . . .
H32B H 1.209693 0.264310 0.289934 0.074 Uiso 1 1 calc R U . . .
H32C H 1.142534 0.284546 0.372166 0.074 Uiso 1 1 calc R U . . .
C33 C 1.07836(15) 0.23618(13) 0.09825(15) 0.0709(7) Uani 1 1 d . . . . .
H33A H 1.024496 0.211383 0.051702 0.106 Uiso 1 1 calc R U . . .
H33B H 1.137671 0.213023 0.096770 0.106 Uiso 1 1 calc R U . . .
H33C H 1.079573 0.281546 0.067549 0.106 Uiso 1 1 calc R U . . .
C34 C 1.07760(10) 0.16945(8) 0.27096(14) 0.0405(4) Uani 1 1 d . . . . .
H34A H 1.076385 0.171285 0.351672 0.061 Uiso 1 1 calc R U . . .
H34B H 1.137866 0.149874 0.263667 0.061 Uiso 1 1 calc R U . . .
H34C H 1.024750 0.141772 0.229324 0.061 Uiso 1 1 calc R U . . .
C17A C 0.3815(15) 0.1016(6) 0.0201(12) 0.069(4) Uani 0.196(6) 1 d . . P D 2
H17D H 0.371081 0.055402 -0.007619 0.103 Uiso 0.196(6) 1 calc R U P D 2
H17E H 0.429142 0.122978 -0.013591 0.103 Uiso 0.196(6) 1 calc R U P D 2
H17F H 0.321680 0.126591 -0.001605 0.103 Uiso 0.196(6) 1 calc R U P D 2
C18A C 0.5134(8) 0.0548(5) 0.1698(15) 0.076(5) Uani 0.196(6) 1 d . . P D 2
H18D H 0.542245 0.050580 0.251666 0.114 Uiso 0.196(6) 1 calc R U P D 2
H18E H 0.558785 0.075890 0.132195 0.114 Uiso 0.196(6) 1 calc R U P D 2
H18F H 0.496653 0.010165 0.137198 0.114 Uiso 0.196(6) 1 calc R U P D 2
C19A C 0.3548(12) 0.0758(6) 0.2104(13) 0.067(5) Uani 0.196(6) 1 d . . P D 2
H19D H 0.323761 0.035738 0.171704 0.101 Uiso 0.196(6) 1 calc R U P D 2
H19E H 0.306639 0.109639 0.214218 0.101 Uiso 0.196(6) 1 calc R U P D 2
H19F H 0.389995 0.064075 0.287734 0.101 Uiso 0.196(6) 1 calc R U P D 2
C27A C 0.8479(9) 0.4336(6) 0.1325(11) 0.035(2) Uani 0.348(14) 1 d . . P E 2
C28A C 0.8406(9) 0.4841(5) 0.2288(14) 0.054(3) Uani 0.348(14) 1 d . . P E 2
H28D H 0.830955 0.529449 0.197108 0.082 Uiso 0.348(14) 1 calc R U P E 2
H28E H 0.899354 0.482686 0.289122 0.082 Uiso 0.348(14) 1 calc R U P E 2
H28F H 0.786760 0.471742 0.260642 0.082 Uiso 0.348(14) 1 calc R U P E 2
C29A C 0.7579(9) 0.4349(7) 0.0372(12) 0.041(3) Uani 0.348(14) 1 d . . P E 2
H29D H 0.703954 0.420397 0.067039 0.061 Uiso 0.348(14) 1 calc R U P E 2
H29E H 0.765157 0.404513 -0.023888 0.061 Uiso 0.348(14) 1 calc R U P E 2
H29F H 0.746650 0.480524 0.007125 0.061 Uiso 0.348(14) 1 calc R U P E 2
C30A C 0.9302(8) 0.4617(3) 0.0837(13) 0.047(2) Uani 0.348(14) 1 d . . P E 2
H30D H 0.913691 0.506810 0.053151 0.070 Uiso 0.348(14) 1 calc R U P E 2
H30E H 0.940138 0.432299 0.022653 0.070 Uiso 0.348(14) 1 calc R U P E 2
H30F H 0.988576 0.463773 0.144582 0.070 Uiso 0.348(14) 1 calc R U P E 2


_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
O1 H1 0.8400 . ?
O1 C7 1.3711(15) . ?
O2 H2 0.8400 . ?
O2 C22 1.3646(15) . ?
O3 C2 1.2040(16) . ?
O4 C2 1.3251(17) . ?
O4 C3 1.469(2) . ?
N1 C1 1.4579(16) . ?
N1 C5 1.4859(15) . ?
N1 C20 1.4784(15) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.5061(18) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C3 C4 1.358(7) . ?
C3 C4A 1.476(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.5053(17) . ?
C6 C7 1.3994(17) . ?
C6 C11 1.3951(18) . ?
C7 C8 1.4054(18) . ?
C8 C9 1.3935(18) . ?
C8 C12 1.5400(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.4001(18) . ?
C10 C11 1.3879(19) . ?
C10 C16 1.5360(17) . ?
C11 H11 0.9500 . ?
C12 C13 1.5402(19) . ?
C12 C14 1.5308(19) . ?
C12 C15 1.5392(18) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.566(3) . ?
C16 C18 1.514(3) . ?
C16 C19 1.515(2) . ?
C16 C17A 1.534(14) . ?
C16 C18A 1.650(10) . ?
C16 C19A 1.378(10) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.5102(17) . ?
C21 C22 1.3992(18) . ?
C21 C26 1.3929(17) . ?
C22 C23 1.4065(18) . ?
C23 C24 1.3947(19) . ?
C23 C27 1.608(5) . ?
C23 C27A 1.417(11) . ?
C24 H24 0.9500 . ?
C24 C25 1.403(2) . ?
C25 C26 1.3879(18) . ?
C25 C31 1.5346(18) . ?
C26 H26 0.9500 . ?
C27 C28 1.532(6) . ?
C27 C29 1.538(4) . ?
C27 C30 1.531(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.536(2) . ?
C31 C33 1.533(2) . ?
C31 C34 1.527(2) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C27A C28A 1.561(13) . ?
C27A C29A 1.519(10) . ?
C27A C30A 1.556(13) . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 0.9800 . ?

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
C7 O1 H1 109.5 . . ?
C22 O2 H2 109.5 . . ?
C2 O4 C3 116.33(12) . . ?
C1 N1 C5 112.14(10) . . ?
C1 N1 C20 111.00(9) . . ?
C20 N1 C5 111.35(10) . . ?
N1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
N1 C1 C2 110.97(10) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
O3 C2 O4 124.00(13) . . ?
O3 C2 C1 125.40(12) . . ?
O4 C2 C1 110.59(11) . . ?
O4 C3 H3AA 109.8 . . ?
O4 C3 H3AB 109.8 . . ?
O4 C3 H3BC 109.6 . . ?
O4 C3 H3BD 109.6 . . ?
O4 C3 C4A 110.4(2) . . ?
H3AA C3 H3AB 108.2 . . ?
H3BC C3 H3BD 108.1 . . ?
C4 C3 O4 109.5(3) . . ?
C4 C3 H3AA 109.8 . . ?
C4 C3 H3AB 109.8 . . ?
C4A C3 H3BC 109.6 . . ?
C4A C3 H3BD 109.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C4A H4AA 109.5 . . ?
C3 C4A H4AB 109.5 . . ?
C3 C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
N1 C5 H5A 109.6 . . ?
N1 C5 H5B 109.6 . . ?
N1 C5 C6 110.28(10) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
C7 C6 C5 119.85(11) . . ?
C11 C6 C5 120.70(11) . . ?
C11 C6 C7 119.40(11) . . ?
O1 C7 C6 121.42(11) . . ?
O1 C7 C8 117.72(10) . . ?
C6 C7 C8 120.86(11) . . ?
C7 C8 C12 121.14(11) . . ?
C9 C8 C7 117.07(11) . . ?
C9 C8 C12 121.78(11) . . ?
C8 C9 H9 118.0 . . ?
C8 C9 C10 123.92(12) . . ?
C10 C9 H9 118.0 . . ?
C9 C10 C16 120.28(12) . . ?
C11 C10 C9 116.82(11) . . ?
C11 C10 C16 122.89(11) . . ?
C6 C11 H11 119.0 . . ?
C10 C11 C6 121.91(11) . . ?
C10 C11 H11 119.0 . . ?
C8 C12 C13 109.37(11) . . ?
C14 C12 C8 111.70(11) . . ?
C14 C12 C13 108.23(12) . . ?
C14 C12 C15 106.97(12) . . ?
C15 C12 C8 110.34(10) . . ?
C15 C12 C13 110.17(11) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C16 C17 108.88(12) . . ?
C10 C16 C18A 106.1(3) . . ?
C18 C16 C10 110.51(13) . . ?
C18 C16 C17 107.75(16) . . ?
C18 C16 C19 109.30(15) . . ?
C19 C16 C10 112.97(13) . . ?
C19 C16 C17 107.25(16) . . ?
C17A C16 C10 110.9(5) . . ?
C17A C16 C18A 102.2(8) . . ?
C19A C16 C10 109.9(4) . . ?
C19A C16 C17A 116.2(8) . . ?
C19A C16 C18A 110.9(9) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.0 . . ?
N1 C20 H20B 109.0 . . ?
N1 C20 C21 112.73(10) . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
C22 C21 C20 120.71(11) . . ?
C26 C21 C20 119.50(11) . . ?
C26 C21 C22 119.66(11) . . ?
O2 C22 C21 120.25(11) . . ?
O2 C22 C23 118.69(11) . . ?
C21 C22 C23 121.06(11) . . ?
C22 C23 C27 120.5(2) . . ?
C22 C23 C27A 121.2(5) . . ?
C24 C23 C22 116.68(12) . . ?
C24 C23 C27 122.8(2) . . ?
C24 C23 C27A 119.6(5) . . ?
C23 C24 H24 118.0 . . ?
C23 C24 C25 124.00(12) . . ?
C25 C24 H24 118.0 . . ?
C24 C25 C31 120.37(12) . . ?
C26 C25 C24 117.02(11) . . ?
C26 C25 C31 122.60(12) . . ?
C21 C26 H26 119.2 . . ?
C25 C26 C21 121.56(12) . . ?
C25 C26 H26 119.2 . . ?
C28 C27 C23 106.0(3) . . ?
C28 C27 C29 109.7(4) . . ?
C29 C27 C23 113.8(4) . . ?
C30 C27 C23 110.8(3) . . ?
C30 C27 C28 109.1(4) . . ?
C30 C27 C29 107.4(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C25 C31 C32 108.68(13) . . ?
C33 C31 C25 109.90(12) . . ?
C33 C31 C32 109.77(15) . . ?
C34 C31 C25 112.12(12) . . ?
C34 C31 C32 108.27(12) . . ?
C34 C31 C33 108.07(14) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C16 C17A H17D 109.5 . . ?
C16 C17A H17E 109.5 . . ?
C16 C17A H17F 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
C16 C18A H18D 109.5 . . ?
C16 C18A H18E 109.5 . . ?
C16 C18A H18F 109.5 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C16 C19A H19D 109.5 . . ?
C16 C19A H19E 109.5 . . ?
C16 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C23 C27A C28A 116.2(7) . . ?
C23 C27A C29A 103.8(8) . . ?
C23 C27A C30A 114.0(8) . . ?
C29A C27A C28A 110.8(9) . . ?
C29A C27A C30A 107.7(7) . . ?
C30A C27A C28A 104.2(8) . . ?
C27A C28A H28D 109.5 . . ?
C27A C28A H28E 109.5 . . ?
C27A C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C27A C29A H29D 109.5 . . ?
C27A C29A H29E 109.5 . . ?
C27A C29A H29F 109.5 . . ?
H29D C29A H29E 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
C27A C30A H30D 109.5 . . ?
C27A C30A H30E 109.5 . . ?
C27A C30A H30F 109.5 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C7 C8 C9 -179.11(10) . . . . ?
O1 C7 C8 C12 0.95(17) . . . . ?
O2 C22 C23 C24 -178.34(12) . . . . ?
O2 C22 C23 C27 -1.0(3) . . . . ?
O2 C22 C23 C27A 19.9(7) . . . . ?
N1 C1 C2 O3 -5.4(2) . . . . ?
N1 C1 C2 O4 175.74(12) . . . . ?
N1 C5 C6 C7 -64.88(14) . . . . ?
N1 C5 C6 C11 112.45(12) . . . . ?
N1 C20 C21 C22 -44.51(15) . . . . ?
N1 C20 C21 C26 139.65(11) . . . . ?
C1 N1 C5 C6 164.53(10) . . . . ?
C1 N1 C20 C21 -69.40(13) . . . . ?
C2 O4 C3 C4 -96.6(3) . . . . ?
C2 O4 C3 C4A -154.9(3) . . . . ?
C3 O4 C2 O3 -1.6(3) . . . . ?
C3 O4 C2 C1 177.23(18) . . . . ?
C5 N1 C1 C2 -77.15(13) . . . . ?
C5 N1 C20 C21 164.89(10) . . . . ?
C5 C6 C7 O1 -3.48(17) . . . . ?
C5 C6 C7 C8 175.92(10) . . . . ?
C5 C6 C11 C10 -177.19(11) . . . . ?
C6 C7 C8 C9 1.47(17) . . . . ?
C6 C7 C8 C12 -178.48(11) . . . . ?
C7 C6 C11 C10 0.16(18) . . . . ?
C7 C8 C9 C10 -0.25(19) . . . . ?
C7 C8 C12 C13 -61.38(15) . . . . ?
C7 C8 C12 C14 178.82(12) . . . . ?
C7 C8 C12 C15 59.96(15) . . . . ?
C8 C9 C10 C11 -0.97(19) . . . . ?
C8 C9 C10 C16 178.49(12) . . . . ?
C9 C8 C12 C13 118.68(13) . . . . ?
C9 C8 C12 C14 -1.12(18) . . . . ?
C9 C8 C12 C15 -119.98(13) . . . . ?
C9 C10 C11 C6 1.01(18) . . . . ?
C9 C10 C16 C17 -58.28(19) . . . . ?
C9 C10 C16 C18 59.88(19) . . . . ?
C9 C10 C16 C19 -177.31(16) . . . . ?
C9 C10 C16 C17A 29.6(9) . . . . ?
C9 C10 C16 C18A 139.8(7) . . . . ?
C9 C10 C16 C19A -100.3(9) . . . . ?
C11 C6 C7 O1 179.16(10) . . . . ?
C11 C6 C7 C8 -1.45(17) . . . . ?
C11 C10 C16 C17 121.14(18) . . . . ?
C11 C10 C16 C18 -120.70(17) . . . . ?
C11 C10 C16 C19 2.1(2) . . . . ?
C11 C10 C16 C17A -151.0(9) . . . . ?
C11 C10 C16 C18A -40.8(7) . . . . ?
C11 C10 C16 C19A 79.2(9) . . . . ?
C12 C8 C9 C10 179.70(12) . . . . ?
C16 C10 C11 C6 -178.43(11) . . . . ?
C20 N1 C1 C2 157.59(10) . . . . ?
C20 N1 C5 C6 -70.41(12) . . . . ?
C20 C21 C22 O2 3.48(18) . . . . ?
C20 C21 C22 C23 -175.81(12) . . . . ?
C20 C21 C26 C25 174.38(11) . . . . ?
C21 C22 C23 C24 0.97(19) . . . . ?
C21 C22 C23 C27 178.3(2) . . . . ?
C21 C22 C23 C27A -160.8(7) . . . . ?
C22 C21 C26 C25 -1.50(18) . . . . ?
C22 C23 C24 C25 -0.6(2) . . . . ?
C22 C23 C27 C28 66.5(4) . . . . ?
C22 C23 C27 C29 -54.2(5) . . . . ?
C22 C23 C27 C30 -175.3(2) . . . . ?
C22 C23 C27A C28A 48.9(10) . . . . ?
C22 C23 C27A C29A -73.0(9) . . . . ?
C22 C23 C27A C30A 170.1(5) . . . . ?
C23 C24 C25 C26 -0.8(2) . . . . ?
C23 C24 C25 C31 -179.20(13) . . . . ?
C24 C23 C27 C28 -116.3(3) . . . . ?
C24 C23 C27 C29 123.0(4) . . . . ?
C24 C23 C27 C30 1.9(4) . . . . ?
C24 C23 C27A C28A -112.3(8) . . . . ?
C24 C23 C27A C29A 125.8(7) . . . . ?
C24 C23 C27A C30A 8.9(8) . . . . ?
C24 C25 C26 C21 1.87(18) . . . . ?
C24 C25 C31 C32 71.00(16) . . . . ?
C24 C25 C31 C33 -49.1(2) . . . . ?
C24 C25 C31 C34 -169.35(13) . . . . ?
C26 C21 C22 O2 179.31(11) . . . . ?
C26 C21 C22 C23 0.01(18) . . . . ?
C26 C25 C31 C32 -107.28(15) . . . . ?
C26 C25 C31 C33 132.59(17) . . . . ?
C26 C25 C31 C34 12.37(19) . . . . ?
C27 C23 C24 C25 -177.9(2) . . . . ?
C31 C25 C26 C21 -179.80(12) . . . . ?
C27A C23 C24 C25 161.5(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 108.5 28.8 '0.5 CH2Cl2'
2 0.000 0.500 0.500 108.5 28.8 '0.5 CH2Cl2'
3 0.130 0.110 0.540 9.0 0.0 ?
4 0.130 0.390 0.040 9.0 0.0 ?
5 0.870 0.610 0.960 9.0 0.0 ?
6 0.870 0.890 0.460 9.0 0.0 ?

_olex2_submission_special_instructions 'No special instructions were received'
