data_exp_1658
_audit_creation_date               2021-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2016/6'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety           'C49 H43 N3 O2 Pd'
_chemical_formula_sum              'C49 H43 N3 O2 Pd'
_chemical_formula_weight           812.26
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
_chemical_oxdiff_formula           'C100 N4 H100 O2 Cl3'
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             45
_space_group_name_H-M_alt          'I b a 2'
_space_group_name_Hall             'I 2 -2c'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 'x+1, -y+1, z+1/2'
 '-x+1, y+1, z+1/2'

_cell_length_a                     34.2146(5)
_cell_length_b                     15.9294(2)
_cell_length_c                     14.1391(2)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       7706.06(18)
_cell_formula_units_Z              8
_cell_measurement_reflns_used      15922
_cell_measurement_temperature      99.9(2)
_cell_measurement_theta_max        71.8540
_cell_measurement_theta_min        3.0540
_shelx_estimated_absorpt_T_max     0.677
_shelx_estimated_absorpt_T_min     0.677
_exptl_absorpt_coefficient_mu      4.232
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.67272
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              blue
_exptl_crystal_colour_primary      blue
_exptl_crystal_density_diffrn      1.400
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               3360
_exptl_crystal_size_max            0.1
_exptl_crystal_size_mid            0.1
_exptl_crystal_size_min            0.1
_exptl_special_details
;
 ?
;
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0311
_diffrn_reflns_av_unetI/netI       0.0278
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  1.000
_diffrn_reflns_limit_h_max         40
_diffrn_reflns_limit_h_min         -40
_diffrn_reflns_limit_k_max         18
_diffrn_reflns_limit_k_min         -18
_diffrn_reflns_limit_l_max         11
_diffrn_reflns_limit_l_min         -16
_diffrn_reflns_number              24293
_diffrn_reflns_point_group_measured_fraction_full  0.786
_diffrn_reflns_point_group_measured_fraction_max  0.786
_diffrn_reflns_theta_full          66.568
_diffrn_reflns_theta_max           66.568
_diffrn_reflns_theta_min           2.583
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        99.9(2)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   8.0697
_diffrn_detector_type              EosS2
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     45.00  83.00   1.00    2.00    --   34.73-125.00  30.00   38
  2  ω     34.00  98.00   1.00    2.00    --   34.73  57.00-180.00   64
  3  ω     37.00  87.00   1.00    2.00    --   34.73-125.00 120.00   50
  4  ω    -21.00  48.00   1.00    2.00    --   34.73 -38.00  60.00   69
  5  ω     20.00 104.00   1.00    2.00    --   34.73  38.00  60.00   84
  6  ω     48.00  86.00   1.00    2.00    --   34.73-125.00-150.00   38
  7  ω     60.00  86.00   1.00    2.00    --   34.73  57.00-150.00   26
  8  ω     10.00 101.00   1.00    2.00    --   34.73  77.00 -60.00   91
  9  ω     27.00 100.00   1.00    2.00    --   34.73  57.00 -90.00   73
 10  ω    103.00 165.00   1.00   16.00    --  105.88 111.00 -90.00   62
 11  ω     51.00 114.00   1.00   16.00    --  105.88 -30.00   0.00   63
 12  ω     79.00 105.00   1.00   16.00    --  105.88 -94.00  90.00   26
 13  ω     64.00 115.00   1.00   16.00    --  105.88-111.00-150.00   51
 14  ω     47.00  97.00   1.00   16.00    --  105.88 -94.00-120.00   50
 15  ω     89.00 114.00   1.00   16.00    --  105.88  45.00 -90.00   25
 16  ω     90.00 171.00   1.00   16.00    --  105.88  77.00   0.00   81
 17  ω     84.00 133.00   1.00   16.00    --  105.88 -77.00   0.00   49
 18  ω     71.00 122.00   1.00   16.00    --  105.88 -61.00 -60.00   51
 19  ω     44.00 122.00   1.00   16.00    --  105.88 -45.00-120.00   78
 20  ω     41.00  89.00   1.00   16.00    --  105.88 -45.00 120.00   48
 21  ω     71.00 107.00   1.00   16.00    --  105.88-111.00  60.00   36
 22  ω    135.00 161.00   1.00   16.00    --  105.88  45.00 -90.00   26
 23  ω     36.00  62.00   1.00   16.00    --  105.88-111.00 -60.00   26
 24  ω     92.00 172.00   1.00   16.00    --  105.88  45.00  60.00   80
 25  ω     53.00 108.00   1.00   16.00    --  105.88 -94.00 -60.00   55
 26  ω     90.00 170.00   1.00   16.00    --  105.88  45.00 -30.00   80
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0228820000
_diffrn_orient_matrix_UB_12        0.0657642000
_diffrn_orient_matrix_UB_13        0.0575255000
_diffrn_orient_matrix_UB_21        0.0325267000
_diffrn_orient_matrix_UB_22        0.0648841000
_diffrn_orient_matrix_UB_23        -0.0184392000
_diffrn_orient_matrix_UB_31        -0.0211449000
_diffrn_orient_matrix_UB_32        0.0286091000
_diffrn_orient_matrix_UB_33        -0.0906326000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.503
_reflns_Friedel_fraction_full      0.552
_reflns_Friedel_fraction_max       0.552
_reflns_number_gt                  5020
_reflns_number_total               5342
_reflns_odcompleteness_completeness  100.00
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       66.49
_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         'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection         'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction          'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.307
_refine_diff_density_min           -0.468
_refine_diff_density_rms           0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 1567 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     -0.029(5)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.038
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       503
_refine_ls_number_reflns           5342
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0256
_refine_ls_R_factor_gt             0.0233
_refine_ls_restrained_S_all        1.038
_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)+(0.0407P)²+0.5811P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0576
_refine_ls_wR_factor_ref           0.0586
_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:
 C16(H16), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C31(H31), C7(H7), C28(H28), C3(H3), C34(H34), C30(H30),
 C12(H12), C23(H23), C2(H2), C43(H43), C29(H29), C21(H21), C45(H45), C27(H27),
 C25(H25), C22(H22), C24(H24), C36(H36)
2.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C39(H39A,H39B,
 H39C), C48(H48A,H48B,H48C), C40(H40A,H40B,H40C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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 0.35761(2) 0.23269(2) 0.45635(2) 0.01499(7) Uani 1 1 d . . . . .
 O1 O 0.26143(7) 0.20071(17) 0.54297(19) 0.0239(5) Uani 1 1 d . . . . .
 H1 H 0.271701 0.163782 0.511117 0.036 Uiso 1 1 calc GR . . . .
 O2 O 0.28889(6) 0.07808(13) 0.4595(3) 0.0217(5) Uani 1 1 d . . . . .
 N1 N 0.30426(7) 0.29299(17) 0.4640(3) 0.0177(6) Uani 1 1 d . . . . .
 N3 N 0.40929(7) 0.17942(15) 0.4554(3) 0.0178(5) Uani 1 1 d . . . . .
 N2 N 0.37981(9) 0.32622(19) 0.3722(2) 0.0196(6) Uani 1 1 d . . . . .
 C8 C 0.41865(12) 0.3976(3) 0.2685(3) 0.0275(9) Uani 1 1 d . . . . .
 H8 H 0.439450 0.411792 0.229313 0.033 Uiso 1 1 calc R . . . .
 C14 C 0.41622(10) 0.1135(2) 0.5100(2) 0.0183(7) Uani 1 1 d . . . . .
 C15 C 0.38378(10) 0.0807(2) 0.5709(3) 0.0183(7) Uani 1 1 d . . . . .
 C16 C 0.34544(10) 0.1283(2) 0.5430(2) 0.0181(7) Uani 1 1 d . . . . .
 H16 H 0.330104 0.144130 0.598716 0.022 Uiso 1 1 calc R . . . .
 C41 C 0.31432(10) 0.5135(2) 0.3597(3) 0.0217(7) Uani 1 1 d . . . . .
 C13 C 0.45593(10) 0.0869(2) 0.4977(3) 0.0206(7) Uani 1 1 d . . . . .
 H13 H 0.468175 0.042092 0.527631 0.025 Uiso 1 1 calc R . . . .
 C31 C 0.42205(11) 0.0365(3) 0.7159(3) 0.0254(8) Uani 1 1 d . . . . .
 H31 H 0.429251 -0.012176 0.683975 0.030 Uiso 1 1 calc R . . . .
 C7 C 0.38504(12) 0.4419(2) 0.2798(3) 0.0259(8) Uani 1 1 d . . . . .
 H7 H 0.378609 0.492183 0.250308 0.031 Uiso 1 1 calc R . . . .
 C9 C 0.41619(10) 0.3254(2) 0.3280(3) 0.0208(7) Uani 1 1 d . . . . .
 C1 C 0.27118(10) 0.2733(2) 0.5099(3) 0.0205(8) Uani 1 1 d . . . . .
 C20 C 0.35627(10) -0.0699(2) 0.6105(3) 0.0218(8) Uani 1 1 d . . . . .
 C19 C 0.37589(10) -0.0124(2) 0.5396(3) 0.0199(7) Uani 1 1 d . . . . .
 H19 H 0.400637 -0.037801 0.519747 0.024 Uiso 1 1 calc R . . . .
 C42 C 0.32818(11) 0.5782(3) 0.4183(3) 0.0256(8) Uani 1 1 d . . . . .
 C28 C 0.40013(11) 0.1800(3) 0.8136(3) 0.0304(9) Uani 1 1 d . . . . .
 H28 H 0.392441 0.227768 0.846554 0.036 Uiso 1 1 calc R . . . .
 C18 C 0.34949(9) -0.0002(2) 0.4511(4) 0.0214(6) Uani 1 1 d . . . . .
 H18A H 0.364809 0.014107 0.395660 0.026 Uiso 1 1 calc R . . . .
 H18B H 0.334132 -0.050016 0.438020 0.026 Uiso 1 1 calc R . . . .
 C3 C 0.26268(10) 0.4088(2) 0.4728(2) 0.0221(8) Uani 1 1 d . . . . .
 H3 H 0.252735 0.462690 0.465413 0.027 Uiso 1 1 calc R . . . .
 C6 C 0.36152(10) 0.3966(2) 0.3455(3) 0.0206(7) Uani 1 1 d . . . . .
 C46 C 0.29337(10) 0.5320(2) 0.2772(3) 0.0227(8) Uani 1 1 d . . . . .
 C34 C 0.52696(12) 0.2735(2) 0.1630(3) 0.0241(8) Uani 1 1 d . . . . .
 H34 H 0.533053 0.248172 0.105613 0.029 Uiso 1 1 calc R . . . .
 C30 C 0.43669(12) 0.0519(3) 0.8056(3) 0.0321(9) Uani 1 1 d . . . . .
 H30 H 0.453987 0.014094 0.833209 0.039 Uiso 1 1 calc R . . . .
 C4 C 0.30003(10) 0.3784(2) 0.4371(2) 0.0197(8) Uani 1 1 d . . . . .
 C12 C 0.47223(10) 0.1403(2) 0.4336(2) 0.0201(8) Uani 1 1 d . . . . .
 H12 H 0.497862 0.138299 0.411846 0.024 Uiso 1 1 calc R . . . .
 C5 C 0.32450(11) 0.4240(2) 0.3826(3) 0.0208(7) Uani 1 1 d . . . . .
 C23 C 0.32015(12) -0.1827(3) 0.7343(3) 0.0304(9) Uani 1 1 d . . . . .
 H23 H 0.308208 -0.220095 0.775737 0.036 Uiso 1 1 calc R . . . .
 C2 C 0.24533(10) 0.3456(2) 0.5180(3) 0.0222(7) Uani 1 1 d . . . . .
 H2 H 0.221319 0.347255 0.548810 0.027 Uiso 1 1 calc R . . . .
 C11 C 0.44344(10) 0.1997(2) 0.4055(3) 0.0184(7) Uani 1 1 d . . . . .
 C43 C 0.31940(11) 0.6608(3) 0.3951(3) 0.0267(8) Uani 1 1 d . . . . .
 H43 H 0.327631 0.703660 0.435041 0.032 Uiso 1 1 calc R . . . .
 C26 C 0.39646(10) 0.0936(2) 0.6731(3) 0.0195(7) Uani 1 1 d . . . . .
 C17 C 0.32404(11) 0.0719(2) 0.4817(2) 0.0198(8) Uani 1 1 d . . . . .
 C32 C 0.48448(10) 0.2854(2) 0.2968(3) 0.0207(7) Uani 1 1 d . . . . .
 C29 C 0.42551(12) 0.1241(3) 0.8547(3) 0.0313(9) Uani 1 1 d . . . . .
 H29 H 0.435241 0.134258 0.915023 0.038 Uiso 1 1 calc R . . . .
 C37 C 0.50992(11) 0.3449(2) 0.3373(3) 0.0269(8) Uani 1 1 d . . . . .
 C21 C 0.32933(11) -0.0418(2) 0.6777(3) 0.0241(8) Uani 1 1 d . . . . .
 H21 H 0.323440 0.015107 0.681437 0.029 Uiso 1 1 calc R . . . .
 C49 C 0.28820(13) 0.7704(2) 0.2910(3) 0.0307(9) Uani 1 1 d . . . . .
 H49A H 0.262824 0.783052 0.316276 0.046 Uiso 1 1 calc GR . . . .
 H49B H 0.287916 0.777992 0.223681 0.046 Uiso 1 1 calc GR . . . .
 H49C H 0.307218 0.807314 0.318656 0.046 Uiso 1 1 calc GR . . . .
 C45 C 0.28627(11) 0.6167(2) 0.2559(3) 0.0248(8) Uani 1 1 d . . . . .
 H45 H 0.272791 0.629893 0.200720 0.030 Uiso 1 1 calc R . . . .
 C27 C 0.38583(11) 0.1655(3) 0.7227(3) 0.0259(8) Uani 1 1 d . . . . .
 H27 H 0.369023 0.204253 0.695017 0.031 Uiso 1 1 calc R . . . .
 C38 C 0.50233(15) 0.3817(3) 0.4333(3) 0.0482(14) Uani 1 1 d . . . . .
 H38A H 0.477397 0.409384 0.433369 0.072 Uiso 1 1 calc GR . . . .
 H38B H 0.522442 0.421630 0.448249 0.072 Uiso 1 1 calc GR . . . .
 H38C H 0.502301 0.337783 0.479781 0.072 Uiso 1 1 calc GR . . . .
 C25 C 0.36445(11) -0.1555(3) 0.6069(3) 0.0258(8) Uani 1 1 d . . . . .
 H25 H 0.382130 -0.175674 0.562391 0.031 Uiso 1 1 calc R . . . .
 C22 C 0.31132(11) -0.0976(3) 0.7386(3) 0.0282(8) Uani 1 1 d . . . . .
 H22 H 0.293241 -0.078121 0.782499 0.034 Uiso 1 1 calc R . . . .
 C35 C 0.55148(11) 0.3355(2) 0.1983(3) 0.0268(8) Uani 1 1 d . . . . .
 C33 C 0.49383(12) 0.2483(2) 0.2109(4) 0.0236(9) Uani 1 1 d . . . . .
 C44 C 0.29860(11) 0.6809(2) 0.3137(3) 0.0251(8) Uani 1 1 d . . . . .
 C10 C 0.44617(11) 0.2673(2) 0.3449(3) 0.0209(8) Uani 1 1 d . . . . .
 C24 C 0.34660(12) -0.2112(3) 0.6688(3) 0.0315(9) Uani 1 1 d . . . . .
 H24 H 0.352567 -0.268077 0.665785 0.038 Uiso 1 1 calc R . . . .
 C47 C 0.27763(13) 0.4638(3) 0.2149(3) 0.0326(9) Uani 1 1 d . . . . .
 H47A H 0.297543 0.422363 0.204517 0.049 Uiso 1 1 calc GR . . . .
 H47B H 0.269758 0.487336 0.155382 0.049 Uiso 1 1 calc GR . . . .
 H47C H 0.255503 0.438028 0.244921 0.049 Uiso 1 1 calc GR . . . .
 C39 C 0.46831(13) 0.1801(3) 0.1690(3) 0.0412(11) Uani 1 1 d . . . . .
 H39A H 0.470973 0.180110 0.101435 0.062 Uiso 1 1 calc GR . . . .
 H39B H 0.441520 0.190284 0.185591 0.062 Uiso 1 1 calc GR . . . .
 H39C H 0.476264 0.126516 0.193541 0.062 Uiso 1 1 calc GR . . . .
 C36 C 0.54297(12) 0.3686(3) 0.2864(3) 0.0312(9) Uani 1 1 d . . . . .
 H36 H 0.559883 0.407992 0.312445 0.037 Uiso 1 1 calc R . . . .
 C48 C 0.35250(15) 0.5590(3) 0.5042(3) 0.0384(11) Uani 1 1 d . . . . .
 H48A H 0.337888 0.523733 0.546423 0.058 Uiso 1 1 calc GR . . . .
 H48B H 0.359144 0.610405 0.535798 0.058 Uiso 1 1 calc GR . . . .
 H48C H 0.375974 0.530609 0.485273 0.058 Uiso 1 1 calc GR . . . .
 C40 C 0.58608(14) 0.3658(3) 0.1415(4) 0.0382(12) Uani 1 1 d . . . . .
 H40A H 0.589204 0.331035 0.086588 0.057 Uiso 1 1 calc GR . . . .
 H40B H 0.609262 0.362812 0.179624 0.057 Uiso 1 1 calc GR . . . .
 H40C H 0.581769 0.422844 0.122241 0.057 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
 Pd1 N1 2.066(3) . ?
 Pd1 N3 1.961(2) . ?
 Pd1 N2 2.052(3) . ?
 Pd1 C16 2.107(3) . ?
 O1 H1 0.8200 . ?
 O1 C1 1.291(5) . ?
 O2 C17 1.247(4) . ?
 N1 C1 1.342(5) . ?
 N1 C4 1.420(4) . ?
 N3 C14 1.326(5) . ?
 N3 C11 1.402(5) . ?
 N2 C9 1.393(5) . ?
 N2 C6 1.339(5) . ?
 C8 H8 0.9300 . ?
 C8 C7 1.358(6) . ?
 C8 C9 1.427(5) . ?
 C14 C15 1.498(5) . ?
 C14 C13 1.433(5) . ?
 C15 C16 1.566(5) . ?
 C15 C19 1.570(5) . ?
 C15 C26 1.522(5) . ?
 C16 H16 0.9800 . ?
 C16 C17 1.447(5) . ?
 C41 C42 1.405(6) . ?
 C41 C46 1.400(5) . ?
 C41 C5 1.503(5) . ?
 C13 H13 0.9300 . ?
 C13 C12 1.362(5) . ?
 C31 H31 0.9300 . ?
 C31 C30 1.386(6) . ?
 C31 C26 1.401(5) . ?
 C7 H7 0.9300 . ?
 C7 C6 1.424(5) . ?
 C9 C10 1.402(5) . ?
 C1 C2 1.456(5) . ?
 C20 C19 1.515(5) . ?
 C20 C21 1.397(6) . ?
 C20 C25 1.394(6) . ?
 C19 H19 0.9800 . ?
 C19 C18 1.556(6) . ?
 C42 C43 1.388(6) . ?
 C42 C48 1.504(6) . ?
 C28 H28 0.9300 . ?
 C28 C29 1.373(6) . ?
 C28 C27 1.394(6) . ?
 C18 H18A 0.9700 . ?
 C18 H18B 0.9700 . ?
 C18 C17 1.504(5) . ?
 C3 H3 0.9300 . ?
 C3 C4 1.457(5) . ?
 C3 C2 1.332(5) . ?
 C6 C5 1.439(5) . ?
 C46 C45 1.404(5) . ?
 C46 C47 1.499(5) . ?
 C34 H34 0.9300 . ?
 C34 C35 1.389(6) . ?
 C34 C33 1.379(6) . ?
 C30 H30 0.9300 . ?
 C30 C29 1.396(7) . ?
 C4 C5 1.350(5) . ?
 C12 H12 0.9300 . ?
 C12 C11 1.422(5) . ?
 C23 H23 0.9300 . ?
 C23 C22 1.390(6) . ?
 C23 C24 1.373(7) . ?
 C2 H2 0.9300 . ?
 C11 C10 1.380(5) . ?
 C43 H43 0.9300 . ?
 C43 C44 1.391(6) . ?
 C26 C27 1.392(6) . ?
 C32 C37 1.408(5) . ?
 C32 C33 1.389(6) . ?
 C32 C10 1.504(5) . ?
 C29 H29 0.9300 . ?
 C37 C38 1.502(6) . ?
 C37 C36 1.393(5) . ?
 C21 H21 0.9300 . ?
 C21 C22 1.382(6) . ?
 C49 H49A 0.9600 . ?
 C49 H49B 0.9600 . ?
 C49 H49C 0.9600 . ?
 C49 C44 1.504(5) . ?
 C45 H45 0.9300 . ?
 C45 C44 1.376(6) . ?
 C27 H27 0.9300 . ?
 C38 H38A 0.9600 . ?
 C38 H38B 0.9600 . ?
 C38 H38C 0.9600 . ?
 C25 H25 0.9300 . ?
 C25 C24 1.387(6) . ?
 C22 H22 0.9300 . ?
 C35 C36 1.383(6) . ?
 C35 C40 1.510(5) . ?
 C33 C39 1.515(6) . ?
 C24 H24 0.9300 . ?
 C47 H47A 0.9600 . ?
 C47 H47B 0.9600 . ?
 C47 H47C 0.9600 . ?
 C39 H39A 0.9600 . ?
 C39 H39B 0.9600 . ?
 C39 H39C 0.9600 . ?
 C36 H36 0.9300 . ?
 C48 H48A 0.9600 . ?
 C48 H48B 0.9600 . ?
 C48 H48C 0.9600 . ?
 C40 H40A 0.9600 . ?
 C40 H40B 0.9600 . ?
 C40 H40C 0.9600 . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 N1 Pd1 C16 99.31(13) . . ?
 N3 Pd1 N1 176.64(15) . . ?
 N3 Pd1 N2 88.65(13) . . ?
 N3 Pd1 C16 80.84(13) . . ?
 N2 Pd1 N1 91.15(12) . . ?
 N2 Pd1 C16 169.46(13) . . ?
 C1 O1 H1 109.5 . . ?
 C1 N1 Pd1 131.5(2) . . ?
 C1 N1 C4 105.5(3) . . ?
 C4 N1 Pd1 121.4(2) . . ?
 C14 N3 Pd1 120.0(2) . . ?
 C14 N3 C11 109.1(3) . . ?
 C11 N3 Pd1 130.9(3) . . ?
 C9 N2 Pd1 125.8(2) . . ?
 C6 N2 Pd1 126.8(2) . . ?
 C6 N2 C9 107.4(3) . . ?
 C7 C8 H8 126.3 . . ?
 C7 C8 C9 107.4(3) . . ?
 C9 C8 H8 126.3 . . ?
 N3 C14 C15 118.6(3) . . ?
 N3 C14 C13 109.4(3) . . ?
 C13 C14 C15 132.0(3) . . ?
 C14 C15 C16 107.9(3) . . ?
 C14 C15 C19 107.1(3) . . ?
 C14 C15 C26 106.7(3) . . ?
 C16 C15 C19 104.0(3) . . ?
 C26 C15 C16 114.4(3) . . ?
 C26 C15 C19 116.3(3) . . ?
 Pd1 C16 H16 111.7 . . ?
 C15 C16 Pd1 111.3(2) . . ?
 C15 C16 H16 111.7 . . ?
 C17 C16 Pd1 104.0(2) . . ?
 C17 C16 C15 105.9(3) . . ?
 C17 C16 H16 111.7 . . ?
 C42 C41 C5 119.4(3) . . ?
 C46 C41 C42 120.6(3) . . ?
 C46 C41 C5 119.8(3) . . ?
 C14 C13 H13 126.7 . . ?
 C12 C13 C14 106.5(3) . . ?
 C12 C13 H13 126.7 . . ?
 C30 C31 H31 119.8 . . ?
 C30 C31 C26 120.4(4) . . ?
 C26 C31 H31 119.8 . . ?
 C8 C7 H7 126.5 . . ?
 C8 C7 C6 107.0(3) . . ?
 C6 C7 H7 126.5 . . ?
 N2 C9 C8 108.1(3) . . ?
 N2 C9 C10 125.7(3) . . ?
 C10 C9 C8 126.1(3) . . ?
 O1 C1 N1 127.0(3) . . ?
 O1 C1 C2 121.5(3) . . ?
 N1 C1 C2 111.5(3) . . ?
 C21 C20 C19 123.3(4) . . ?
 C25 C20 C19 118.6(3) . . ?
 C25 C20 C21 118.1(4) . . ?
 C15 C19 H19 108.8 . . ?
 C20 C19 C15 117.4(3) . . ?
 C20 C19 H19 108.8 . . ?
 C20 C19 C18 110.5(3) . . ?
 C18 C19 C15 102.0(3) . . ?
 C18 C19 H19 108.8 . . ?
 C41 C42 C48 120.9(4) . . ?
 C43 C42 C41 118.9(4) . . ?
 C43 C42 C48 120.2(4) . . ?
 C29 C28 H28 119.9 . . ?
 C29 C28 C27 120.3(4) . . ?
 C27 C28 H28 119.9 . . ?
 C19 C18 H18A 111.5 . . ?
 C19 C18 H18B 111.5 . . ?
 H18A C18 H18B 109.3 . . ?
 C17 C18 C19 101.6(4) . . ?
 C17 C18 H18A 111.5 . . ?
 C17 C18 H18B 111.5 . . ?
 C4 C3 H3 126.1 . . ?
 C2 C3 H3 126.1 . . ?
 C2 C3 C4 107.8(3) . . ?
 N2 C6 C7 110.1(3) . . ?
 N2 C6 C5 124.2(3) . . ?
 C7 C6 C5 125.6(3) . . ?
 C41 C46 C45 118.0(4) . . ?
 C41 C46 C47 121.4(3) . . ?
 C45 C46 C47 120.5(4) . . ?
 C35 C34 H34 119.1 . . ?
 C33 C34 H34 119.1 . . ?
 C33 C34 C35 121.8(4) . . ?
 C31 C30 H30 119.9 . . ?
 C31 C30 C29 120.1(4) . . ?
 C29 C30 H30 119.9 . . ?
 N1 C4 C3 108.3(3) . . ?
 C5 C4 N1 127.3(3) . . ?
 C5 C4 C3 124.3(3) . . ?
 C13 C12 H12 125.7 . . ?
 C13 C12 C11 108.5(3) . . ?
 C11 C12 H12 125.7 . . ?
 C6 C5 C41 114.4(3) . . ?
 C4 C5 C41 119.3(3) . . ?
 C4 C5 C6 126.2(3) . . ?
 C22 C23 H23 120.2 . . ?
 C24 C23 H23 120.2 . . ?
 C24 C23 C22 119.7(4) . . ?
 C1 C2 H2 126.6 . . ?
 C3 C2 C1 106.8(3) . . ?
 C3 C2 H2 126.6 . . ?
 N3 C11 C12 106.5(3) . . ?
 C10 C11 N3 123.3(3) . . ?
 C10 C11 C12 130.2(3) . . ?
 C42 C43 H43 119.2 . . ?
 C42 C43 C44 121.6(4) . . ?
 C44 C43 H43 119.2 . . ?
 C31 C26 C15 120.1(3) . . ?
 C27 C26 C15 121.0(3) . . ?
 C27 C26 C31 118.7(4) . . ?
 O2 C17 C16 126.1(3) . . ?
 O2 C17 C18 123.1(3) . . ?
 C16 C17 C18 110.7(3) . . ?
 C37 C32 C10 118.9(3) . . ?
 C33 C32 C37 120.0(3) . . ?
 C33 C32 C10 121.0(3) . . ?
 C28 C29 C30 119.8(4) . . ?
 C28 C29 H29 120.1 . . ?
 C30 C29 H29 120.1 . . ?
 C32 C37 C38 121.6(4) . . ?
 C36 C37 C32 118.3(4) . . ?
 C36 C37 C38 120.1(4) . . ?
 C20 C21 H21 119.6 . . ?
 C22 C21 C20 120.8(4) . . ?
 C22 C21 H21 119.6 . . ?
 H49A C49 H49B 109.5 . . ?
 H49A C49 H49C 109.5 . . ?
 H49B C49 H49C 109.5 . . ?
 C44 C49 H49A 109.5 . . ?
 C44 C49 H49B 109.5 . . ?
 C44 C49 H49C 109.5 . . ?
 C46 C45 H45 118.9 . . ?
 C44 C45 C46 122.2(4) . . ?
 C44 C45 H45 118.9 . . ?
 C28 C27 H27 119.7 . . ?
 C26 C27 C28 120.6(4) . . ?
 C26 C27 H27 119.7 . . ?
 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 . . ?
 C20 C25 H25 119.5 . . ?
 C24 C25 C20 120.9(4) . . ?
 C24 C25 H25 119.5 . . ?
 C23 C22 H22 119.9 . . ?
 C21 C22 C23 120.2(4) . . ?
 C21 C22 H22 119.9 . . ?
 C34 C35 C40 120.7(4) . . ?
 C36 C35 C34 117.9(4) . . ?
 C36 C35 C40 121.5(4) . . ?
 C34 C33 C32 119.7(4) . . ?
 C34 C33 C39 119.4(4) . . ?
 C32 C33 C39 120.9(4) . . ?
 C43 C44 C49 121.1(4) . . ?
 C45 C44 C43 118.5(4) . . ?
 C45 C44 C49 120.3(4) . . ?
 C9 C10 C32 115.7(3) . . ?
 C11 C10 C9 124.9(3) . . ?
 C11 C10 C32 119.3(3) . . ?
 C23 C24 C25 120.3(4) . . ?
 C23 C24 H24 119.8 . . ?
 C25 C24 H24 119.8 . . ?
 C46 C47 H47A 109.5 . . ?
 C46 C47 H47B 109.5 . . ?
 C46 C47 H47C 109.5 . . ?
 H47A C47 H47B 109.5 . . ?
 H47A C47 H47C 109.5 . . ?
 H47B C47 H47C 109.5 . . ?
 C33 C39 H39A 109.5 . . ?
 C33 C39 H39B 109.5 . . ?
 C33 C39 H39C 109.5 . . ?
 H39A C39 H39B 109.5 . . ?
 H39A C39 H39C 109.5 . . ?
 H39B C39 H39C 109.5 . . ?
 C37 C36 H36 118.9 . . ?
 C35 C36 C37 122.2(4) . . ?
 C35 C36 H36 118.9 . . ?
 C42 C48 H48A 109.5 . . ?
 C42 C48 H48B 109.5 . . ?
 C42 C48 H48C 109.5 . . ?
 H48A C48 H48B 109.5 . . ?
 H48A C48 H48C 109.5 . . ?
 H48B C48 H48C 109.5 . . ?
 C35 C40 H40A 109.5 . . ?
 C35 C40 H40B 109.5 . . ?
 C35 C40 H40C 109.5 . . ?
 H40A C40 H40B 109.5 . . ?
 H40A C40 H40C 109.5 . . ?
 H40B C40 H40C 109.5 . . ?

_olex2_date_sample_data_collection  2021-07-06
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.549
_oxdiff_exptl_absorpt_empirical_full_min  0.729
