#------------------------------------------------------------------------------
#$Date: 2021-11-16 02:13:25 +0200 (Tue, 16 Nov 2021) $
#$Revision: 270672 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/88/7708827.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708827
loop_
_publ_author_name
'Fazekas, Eszter'
'Jenkins, David T.'
'Forbes, Andrew A.'
'Gallagher, Brendan'
'Rosair, Georgina'
'McIntosh, Ruaraidh D.'
_publ_section_title
;
 Amino acid-derived bisphenolate palladium complexes as C-C coupling
 catalysts
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03068J
_journal_year                    2021
_chemical_formula_moiety         'C38 H62 N2 O4 Pd, C3 H7.5'
_chemical_formula_sum            'C41 H69.5 N2 O4 Pd'
_chemical_formula_weight         760.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.3384(7)
_cell_length_b                   9.7533(2)
_cell_length_c                   31.2674(8)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      59.871
_cell_measurement_theta_min      4.085
_cell_volume                     8289.3(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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)'
_diffrn_ambient_temperature      100.0
_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_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_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_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_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.219
_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
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.057
_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_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0271
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5449
_reflns_number_total             6054
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03068j2.cif
_cod_data_source_block           131bg14_0m
_cod_original_formula_sum        'C41 H69.50 N2 O4 Pd'
_cod_database_code               7708827
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.480
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
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 . .
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'
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_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_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) . . . . ?
