# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_cjr-20220712
_database_code_depnum_ccdc_archive 'CCDC 2191732'
loop_
_audit_author_name
_audit_author_address
'Jie Zhang'
;Henan Normal University
China
;
_audit_update_record             
;
2022-07-21 deposited with the CCDC.	2022-11-02 downloaded from the CCDC.
;
_audit_creation_date             2022-07-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        tBu-PNCNP-Pd-H
_chemical_formula_moiety         'C22 H42 N2 P2 Pd'
_chemical_formula_sum            'C22 H42 N2 P2 Pd'
_chemical_formula_weight         502.91
_chemical_melting_point          ?
_chemical_oxdiff_formula         'P1 N1 C1 Pd1'
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'
P P 0.2955 0.4335 '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           61
_space_group_name_H-M_alt        'P b c a'
_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'
'-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                   11.4139(2)
_cell_length_b                   15.3554(3)
_cell_length_c                   28.0400(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4914.43(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5639
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.2310
_cell_measurement_theta_min      5.0010
_shelx_estimated_absorpt_T_max   0.867
_shelx_estimated_absorpt_T_min   0.867
_exptl_absorpt_coefficient_mu    7.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12651
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.518
_diffrn_reflns_theta_min         4.997
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  32.00   1.00    4.16    --  -35.62  76.00  56.00   42
  2  ω    -92.00 -19.00   1.00    4.16    --  -35.62 -76.00 -70.00   73
  3  ω     -4.00  23.00   1.00    4.16    --   35.62 -92.00-169.00   27
  4  ω     44.00  86.00   1.00   16.65    --  107.12 -92.00-169.00   42
  5  ω     45.00 118.00   1.00   16.65    --  107.12 -57.00  58.00   73
  6  ω     81.00 173.00   1.00   16.65    --  107.12  76.00  56.00   92
  7  ω    -41.00  34.00   1.00    4.16    --  -35.62  38.00 -90.00   75
  8  ω     59.00 107.00   1.00    4.16    --   35.62 178.00 -30.00   48
  9  ω     85.00 119.00   1.00   16.65    --  107.12 -77.00-150.00   34
 10  ω     40.00  83.00   1.00   16.65    --  107.12 -77.00-150.00   43
 11  ω     55.00 128.00   1.00   16.65    --  107.12 -30.00 -90.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0580759000
_diffrn_orient_matrix_UB_12      -0.0827109000
_diffrn_orient_matrix_UB_13      -0.0201076000
_diffrn_orient_matrix_UB_21      -0.0711008000
_diffrn_orient_matrix_UB_22      0.0099680000
_diffrn_orient_matrix_UB_23      -0.0463904000
_diffrn_orient_matrix_UB_31      0.0990458000
_diffrn_orient_matrix_UB_32      0.0556560000
_diffrn_orient_matrix_UB_33      -0.0216112000
_diffrn_oxdiff_digest_frames     
;
01023684dba86bc3f3950d16373bab004900027790f
;
_diffrn_oxdiff_digest_hkl        
;
0133ec68b2e7388f8b358c863b1ec771c9b60d
;
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3965
_reflns_number_total             4655
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.534
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4655
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0455
_refine_ls_restrained_S_all      1.067
_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)+(0.0616P)²+7.8607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1222
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C8(H8A,H8B,
 H8C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C14(H14A,H14B,
 H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C20(H20A,
 H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.58579(2) 0.66293(2) 0.38569(2) 0.01802(12) Uani 1 1 d . . . . .
P2 P 0.75841(8) 0.63200(6) 0.34966(3) 0.0163(2) Uani 1 1 d . . . . .
P1 P 0.39308(9) 0.67113(6) 0.40449(4) 0.0188(2) Uani 1 1 d . . . . .
N2 N 0.7180(3) 0.5660(2) 0.30375(12) 0.0215(7) Uani 1 1 d . . . . .
N1 N 0.3294(3) 0.6072(2) 0.36195(13) 0.0243(7) Uani 1 1 d . . . . .
C1 C 0.5234(4) 0.5809(2) 0.33365(14) 0.0204(8) Uani 1 1 d . . . . .
C6 C 0.5991(4) 0.5420(3) 0.30128(14) 0.0192(8) Uani 1 1 d . . . . .
C5 C 0.5584(4) 0.4798(2) 0.26821(14) 0.0210(8) Uani 1 1 d . . . . .
H5 H 0.609612 0.453670 0.246744 0.025 Uiso 1 1 calc R . . . .
C2 C 0.4041(3) 0.5614(3) 0.33102(14) 0.0188(8) Uani 1 1 d . . . . .
C3 C 0.3622(4) 0.4985(3) 0.29935(14) 0.0225(8) Uani 1 1 d . . . . .
H3 H 0.283252 0.483490 0.298986 0.027 Uiso 1 1 calc R . . . .
C19 C 0.3463(4) 0.6186(3) 0.46170(15) 0.0262(9) Uani 1 1 d . . . . .
C4 C 0.4407(4) 0.4587(2) 0.26843(15) 0.0226(8) Uani 1 1 d . . . . .
H4 H 0.413398 0.416682 0.247295 0.027 Uiso 1 1 calc R . . . .
C7 C 0.8318(4) 0.7261(2) 0.31963(15) 0.0211(8) Uani 1 1 d . . . . .
C15 C 0.3263(4) 0.7809(3) 0.39472(17) 0.0257(9) Uani 1 1 d . . . . .
C11 C 0.8621(4) 0.5639(3) 0.38562(14) 0.0209(8) Uani 1 1 d . . . . .
C10 C 0.8850(4) 0.7860(3) 0.35777(17) 0.0272(9) Uani 1 1 d . . . . .
H10A H 0.829109 0.794839 0.382890 0.041 Uiso 1 1 calc GR . . . .
H10B H 0.904729 0.841020 0.343664 0.041 Uiso 1 1 calc GR . . . .
H10C H 0.954385 0.759519 0.370593 0.041 Uiso 1 1 calc GR . . . .
C13 C 0.8805(5) 0.6054(3) 0.43492(16) 0.0325(10) Uani 1 1 d . . . . .
H13A H 0.920677 0.659924 0.431342 0.049 Uiso 1 1 calc GR . . . .
H13B H 0.926473 0.567058 0.454448 0.049 Uiso 1 1 calc GR . . . .
H13C H 0.805853 0.615134 0.449768 0.049 Uiso 1 1 calc GR . . . .
C21 C 0.3860(5) 0.5236(3) 0.45674(18) 0.0341(10) Uani 1 1 d . . . . .
H21A H 0.345828 0.497008 0.430412 0.051 Uiso 1 1 calc GR . . . .
H21B H 0.367947 0.492524 0.485536 0.051 Uiso 1 1 calc GR . . . .
H21C H 0.468911 0.521781 0.451185 0.051 Uiso 1 1 calc GR . . . .
C8 C 0.9239(4) 0.7014(3) 0.28226(17) 0.0300(10) Uani 1 1 d . . . . .
H8A H 0.989857 0.674834 0.297758 0.045 Uiso 1 1 calc GR . . . .
H8B H 0.949100 0.752772 0.265682 0.045 Uiso 1 1 calc GR . . . .
H8C H 0.890478 0.661049 0.259913 0.045 Uiso 1 1 calc GR . . . .
C12 C 0.9809(4) 0.5473(3) 0.36219(17) 0.0314(10) Uani 1 1 d . . . . .
H12A H 0.969206 0.524425 0.330688 0.047 Uiso 1 1 calc GR . . . .
H12B H 1.024382 0.506146 0.380899 0.047 Uiso 1 1 calc GR . . . .
H12C H 1.023697 0.601023 0.360255 0.047 Uiso 1 1 calc GR . . . .
C9 C 0.7319(4) 0.7744(3) 0.29439(18) 0.0327(10) Uani 1 1 d . . . . .
H9A H 0.698044 0.737347 0.270526 0.049 Uiso 1 1 calc GR . . . .
H9B H 0.762112 0.826134 0.279557 0.049 Uiso 1 1 calc GR . . . .
H9C H 0.673050 0.790151 0.317282 0.049 Uiso 1 1 calc GR . . . .
C18 C 0.3560(5) 0.8413(3) 0.43651(19) 0.0356(11) Uani 1 1 d . . . . .
H18A H 0.312528 0.823667 0.464183 0.053 Uiso 1 1 calc GR . . . .
H18B H 0.335711 0.900081 0.428328 0.053 Uiso 1 1 calc GR . . . .
H18C H 0.438375 0.837933 0.443194 0.053 Uiso 1 1 calc GR . . . .
C14 C 0.7988(5) 0.4764(3) 0.39311(19) 0.0362(11) Uani 1 1 d . . . . .
H14A H 0.722831 0.486727 0.406698 0.054 Uiso 1 1 calc GR . . . .
H14B H 0.843859 0.440504 0.414311 0.054 Uiso 1 1 calc GR . . . .
H14C H 0.790135 0.447342 0.362994 0.054 Uiso 1 1 calc GR . . . .
C17 C 0.1934(4) 0.7788(3) 0.3861(2) 0.0376(12) Uani 1 1 d . . . . .
H17A H 0.175939 0.738133 0.361118 0.056 Uiso 1 1 calc GR . . . .
H17B H 0.167015 0.835800 0.376990 0.056 Uiso 1 1 calc GR . . . .
H17C H 0.154285 0.761280 0.414852 0.056 Uiso 1 1 calc GR . . . .
C16 C 0.3858(5) 0.8149(3) 0.34905(18) 0.0350(11) Uani 1 1 d . . . . .
H16A H 0.468426 0.820980 0.354503 0.052 Uiso 1 1 calc GR . . . .
H16B H 0.353163 0.870430 0.340681 0.052 Uiso 1 1 calc GR . . . .
H16C H 0.372862 0.774392 0.323493 0.052 Uiso 1 1 calc GR . . . .
C22 C 0.4111(5) 0.6600(3) 0.50379(17) 0.0345(11) Uani 1 1 d . . . . .
H22A H 0.493636 0.660980 0.497256 0.052 Uiso 1 1 calc GR . . . .
H22B H 0.396765 0.626553 0.532119 0.052 Uiso 1 1 calc GR . . . .
H22C H 0.383475 0.718464 0.508389 0.052 Uiso 1 1 calc GR . . . .
C20 C 0.2138(5) 0.6208(4) 0.4704(2) 0.0457(14) Uani 1 1 d . . . . .
H20A H 0.190228 0.679157 0.478084 0.069 Uiso 1 1 calc GR . . . .
H20B H 0.194588 0.582767 0.496422 0.069 Uiso 1 1 calc GR . . . .
H20C H 0.173644 0.601892 0.442169 0.069 Uiso 1 1 calc GR . . . .
H1 H 0.257(5) 0.597(3) 0.3618(19) 0.025(13) Uiso 1 1 d . . . . .
H2 H 0.761(5) 0.549(4) 0.287(2) 0.030(15) Uiso 1 1 d . . . . .
H H 0.629(6) 0.728(4) 0.428(2) 0.056(19) Uiso 1 1 d . . . . .


_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 P2 2.2646(10) . ?
Pd1 P1 2.2653(10) . ?
Pd1 C1 2.055(4) . ?
Pd1 H 1.62(7) . ?
P2 N2 1.702(3) . ?
P2 C7 1.870(4) . ?
P2 C11 1.874(4) . ?
P1 N1 1.707(4) . ?
P1 C19 1.873(4) . ?
P1 C15 1.870(4) . ?
N2 C6 1.408(5) . ?
N2 H2 0.74(6) . ?
N1 C2 1.405(5) . ?
N1 H1 0.84(5) . ?
C1 C6 1.388(6) . ?
C1 C2 1.396(6) . ?
C6 C5 1.410(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.382(6) . ?
C2 C3 1.396(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.389(6) . ?
C19 C21 1.534(6) . ?
C19 C22 1.531(6) . ?
C19 C20 1.532(7) . ?
C4 H4 0.9300 . ?
C7 C10 1.536(6) . ?
C7 C8 1.532(6) . ?
C7 C9 1.534(6) . ?
C15 C18 1.532(6) . ?
C15 C17 1.537(6) . ?
C15 C16 1.541(7) . ?
C11 C13 1.537(6) . ?
C11 C12 1.528(6) . ?
C11 C14 1.540(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 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
P2 Pd1 P1 163.78(4) . . ?
P2 Pd1 H 101(2) . . ?
P1 Pd1 H 95(2) . . ?
C1 Pd1 P2 81.73(12) . . ?
C1 Pd1 P1 82.11(12) . . ?
C1 Pd1 H 177(2) . . ?
N2 P2 Pd1 103.09(13) . . ?
N2 P2 C7 103.92(18) . . ?
N2 P2 C11 104.23(18) . . ?
C7 P2 Pd1 115.39(13) . . ?
C7 P2 C11 112.99(19) . . ?
C11 P2 Pd1 115.23(13) . . ?
N1 P1 Pd1 102.64(13) . . ?
N1 P1 C19 103.3(2) . . ?
N1 P1 C15 104.0(2) . . ?
C19 P1 Pd1 116.88(15) . . ?
C15 P1 Pd1 114.30(15) . . ?
C15 P1 C19 113.4(2) . . ?
P2 N2 H2 122(4) . . ?
C6 N2 P2 117.0(3) . . ?
C6 N2 H2 121(4) . . ?
P1 N1 H1 122(4) . . ?
C2 N1 P1 117.5(3) . . ?
C2 N1 H1 120(4) . . ?
C6 C1 Pd1 120.8(3) . . ?
C6 C1 C2 118.7(4) . . ?
C2 C1 Pd1 120.5(3) . . ?
N2 C6 C5 121.8(4) . . ?
C1 C6 N2 117.1(4) . . ?
C1 C6 C5 121.1(4) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 C6 118.4(4) . . ?
C4 C5 H5 120.8 . . ?
C1 C2 N1 116.8(4) . . ?
C1 C2 C3 121.1(4) . . ?
C3 C2 N1 122.1(4) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.7(4) . . ?
C4 C3 H3 120.7 . . ?
C21 C19 P1 104.4(3) . . ?
C22 C19 P1 110.1(3) . . ?
C22 C19 C21 108.8(4) . . ?
C22 C19 C20 110.2(4) . . ?
C20 C19 P1 114.1(3) . . ?
C20 C19 C21 109.1(4) . . ?
C5 C4 C3 121.8(4) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C10 C7 P2 109.0(3) . . ?
C8 C7 P2 115.1(3) . . ?
C8 C7 C10 110.7(4) . . ?
C8 C7 C9 108.3(4) . . ?
C9 C7 P2 104.4(3) . . ?
C9 C7 C10 109.0(3) . . ?
C18 C15 P1 110.1(3) . . ?
C18 C15 C17 110.5(4) . . ?
C18 C15 C16 109.5(4) . . ?
C17 C15 P1 114.0(3) . . ?
C17 C15 C16 108.1(4) . . ?
C16 C15 P1 104.3(3) . . ?
C13 C11 P2 109.8(3) . . ?
C13 C11 C14 107.7(4) . . ?
C12 C11 P2 114.9(3) . . ?
C12 C11 C13 109.5(4) . . ?
C12 C11 C14 109.3(4) . . ?
C14 C11 P2 105.3(3) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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 . . ?
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 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
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 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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 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 . . ?
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 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 . . ?
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 . . ?
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 . . ?

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 P2 N2 C6 -4.8(3) . . . . ?
Pd1 P2 C7 C10 74.2(3) . . . . ?
Pd1 P2 C7 C8 -160.7(3) . . . . ?
Pd1 P2 C7 C9 -42.1(3) . . . . ?
Pd1 P2 C11 C13 -52.9(3) . . . . ?
Pd1 P2 C11 C12 -176.9(3) . . . . ?
Pd1 P2 C11 C14 62.8(3) . . . . ?
Pd1 P1 N1 C2 5.8(3) . . . . ?
Pd1 P1 C19 C21 -56.9(3) . . . . ?
Pd1 P1 C19 C22 59.8(3) . . . . ?
Pd1 P1 C19 C20 -175.8(3) . . . . ?
Pd1 P1 C15 C18 -80.3(3) . . . . ?
Pd1 P1 C15 C17 154.8(3) . . . . ?
Pd1 P1 C15 C16 37.1(3) . . . . ?
Pd1 C1 C6 N2 -4.3(5) . . . . ?
Pd1 C1 C6 C5 174.4(3) . . . . ?
Pd1 C1 C2 N1 6.5(5) . . . . ?
Pd1 C1 C2 C3 -172.8(3) . . . . ?
P2 N2 C6 C1 6.1(5) . . . . ?
P2 N2 C6 C5 -172.5(3) . . . . ?
P1 N1 C2 C1 -8.2(5) . . . . ?
P1 N1 C2 C3 171.1(3) . . . . ?
N2 P2 C7 C10 -173.7(3) . . . . ?
N2 P2 C7 C8 -48.6(4) . . . . ?
N2 P2 C7 C9 70.0(3) . . . . ?
N2 P2 C11 C13 -165.1(3) . . . . ?
N2 P2 C11 C12 70.9(3) . . . . ?
N2 P2 C11 C14 -49.4(3) . . . . ?
N2 C6 C5 C4 179.0(4) . . . . ?
N1 P1 C19 C21 55.0(3) . . . . ?
N1 P1 C19 C22 171.6(3) . . . . ?
N1 P1 C19 C20 -64.0(4) . . . . ?
N1 P1 C15 C18 168.6(3) . . . . ?
N1 P1 C15 C17 43.7(4) . . . . ?
N1 P1 C15 C16 -74.0(3) . . . . ?
N1 C2 C3 C4 177.2(4) . . . . ?
C1 C6 C5 C4 0.5(6) . . . . ?
C1 C2 C3 C4 -3.5(6) . . . . ?
C6 C1 C2 N1 -175.2(4) . . . . ?
C6 C1 C2 C3 5.5(6) . . . . ?
C6 C5 C4 C3 1.6(6) . . . . ?
C2 C1 C6 N2 177.4(4) . . . . ?
C2 C1 C6 C5 -3.9(6) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C19 P1 N1 C2 -116.1(3) . . . . ?
C19 P1 C15 C18 57.1(4) . . . . ?
C19 P1 C15 C17 -67.7(4) . . . . ?
C19 P1 C15 C16 174.5(3) . . . . ?
C7 P2 N2 C6 -125.5(3) . . . . ?
C7 P2 C11 C13 82.8(3) . . . . ?
C7 P2 C11 C12 -41.2(4) . . . . ?
C7 P2 C11 C14 -161.6(3) . . . . ?
C15 P1 N1 C2 125.2(3) . . . . ?
C15 P1 C19 C21 166.9(3) . . . . ?
C15 P1 C19 C22 -76.5(4) . . . . ?
C15 P1 C19 C20 48.0(4) . . . . ?
C11 P2 N2 C6 115.9(3) . . . . ?
C11 P2 C7 C10 -61.4(3) . . . . ?
C11 P2 C7 C8 63.7(4) . . . . ?
C11 P2 C7 C9 -177.7(3) . . . . ?

_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 4.429
_oxdiff_exptl_absorpt_empirical_full_min 0.577
####################################################################### 
# 
# 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_cjr-20211203
_database_code_depnum_ccdc_archive 'CCDC 2191735'
loop_
_audit_author_name
_audit_author_address
'Jie Zhang'
;Henan Normal University
China
;
_audit_update_record             
;
2022-10-25 deposited with the CCDC.	2022-11-02 downloaded from the CCDC.
;
_audit_creation_date             2022-10-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        tBu-PNCNP-Pd-NHCOCH3
_chemical_formula_moiety         'C24 H45 N3 O P2 Pd, 2(C2 H3 N)'
_chemical_formula_sum            'C28 H51 N5 O P2 Pd'
_chemical_formula_weight         642.07
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 P1 N1 Pd1'
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'
P P 0.2955 0.4335 '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                   11.71590(10)
_cell_length_b                   14.45290(10)
_cell_length_c                   19.6929(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.1230(10)
_cell_angle_gamma                90
_cell_volume                     3321.25(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.3790
_cell_measurement_theta_min      3.7960
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.552
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14789
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.500
_diffrn_reflns_theta_min         3.788
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  -3.00   1.00    1.00    --  -35.62  61.00 -46.00   49
  2  ω   -103.00 -31.00   1.00    1.00    --  -35.62 -61.00 174.00   72
  3  ω     76.00 102.00   1.00    1.00    --   35.62  61.00 -46.00   26
  4  ω    -13.00  12.00   1.00    1.00    --   35.62 -61.00 174.00   25
  5  ω    107.00 132.00   1.00    1.16    --  107.12  61.00 -46.00   25
  6  ω     41.00 124.00   1.00    1.16    --  107.12 -61.00 174.00   83
  7  ω    -74.00 -35.00   1.00    1.00    --  -35.62-178.00-120.00   39
  8  ω     16.00  73.00   1.00    1.00    --   35.62 -99.00-150.00   57
  9  ω     68.00 107.00   1.00    1.00    --   35.62 178.00-150.00   39
 10  ω     80.00 107.00   1.00    1.00    --   35.62-178.00-150.00   27
 11  ω    -34.00  41.00   1.00    1.00    --   35.62 -38.00  60.00   75
 12  ω     75.00 105.00   1.00    1.16    --  107.12 -95.00 -90.00   30
 13  ω     37.00 113.00   1.00    1.16    --  107.12-111.00-150.00   76
 14  ω    103.00 159.00   1.00    1.16    --  107.12 111.00 150.00   56
 15  ω     40.00  78.00   1.00    1.16    --  107.12 -61.00  30.00   38
 16  ω     90.00 174.00   1.00    1.16    --  107.12  61.00 -60.00   84
 17  ω     90.00 173.00   1.00    1.16    --  107.12  61.00 -90.00   83
 18  ω     82.00 109.00   1.00    1.16    --  107.12 -95.00  30.00   27
 19  ω     64.00  97.00   1.00    1.16    --  107.12 -95.00 120.00   33
 20  ω     64.00 111.00   1.00    1.16    --  107.12-111.00  30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0571891000
_diffrn_orient_matrix_UB_12      -0.0335467000
_diffrn_orient_matrix_UB_13      0.0691219000
_diffrn_orient_matrix_UB_21      -0.0994029000
_diffrn_orient_matrix_UB_22      -0.0684257000
_diffrn_orient_matrix_UB_23      0.0062722000
_diffrn_orient_matrix_UB_31      0.0654501000
_diffrn_orient_matrix_UB_32      -0.0745242000
_diffrn_orient_matrix_UB_33      -0.0367419000
_diffrn_oxdiff_digest_frames     
;
01122d244cb9873a6217dc3df1e9c2956f0002729d4
;
_diffrn_oxdiff_digest_hkl        
;
0125bee59f62fdb4a7c05e123eeb630ecd9748
;
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5840
_reflns_number_total             6346
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      1.071
_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)+(0.0387P)²+3.1646P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0849
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C22(H22A,
 H22B,H22C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C),
 C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C11(H11A,H11B,H11C), C26(H26A,H26B,
 H26C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.72273(2) 0.27963(2) 0.72970(2) 0.01958(7) Uani 1 1 d . . . . .
P1 P 0.58771(6) 0.19488(4) 0.78062(3) 0.02137(14) Uani 1 1 d . . . . .
P2 P 0.85889(6) 0.32162(5) 0.65783(3) 0.02398(15) Uani 1 1 d . . . . .
O1 O 0.63725(19) 0.48746(15) 0.77180(11) 0.0375(5) Uani 1 1 d . . . . .
N3 N 0.7633(2) 0.37651(16) 0.80834(12) 0.0251(5) Uani 1 1 d . . . . .
N1 N 0.5325(2) 0.12677(18) 0.71684(13) 0.0296(5) Uani 1 1 d . . . . .
N2 N 0.8261(2) 0.25277(18) 0.58986(13) 0.0301(5) Uani 1 1 d . . . . .
C1 C 0.6810(2) 0.18890(18) 0.65394(13) 0.0232(5) Uani 1 1 d . . . . .
C6 C 0.5917(2) 0.12475(19) 0.65837(14) 0.0249(5) Uani 1 1 d . . . . .
C2 C 0.7377(2) 0.18890(19) 0.59408(14) 0.0254(5) Uani 1 1 d . . . . .
C7 C 0.7164(2) 0.45773(19) 0.81335(14) 0.0270(6) Uani 1 1 d . . . . .
C3 C 0.7069(3) 0.1280(2) 0.54049(15) 0.0316(6) Uani 1 1 d . . . . .
H3A H 0.745500 0.129630 0.500074 0.038 Uiso 1 1 calc R . . . .
C5 C 0.5621(2) 0.0620(2) 0.60571(15) 0.0315(6) Uani 1 1 d . . . . .
H5 H 0.503441 0.017582 0.609988 0.038 Uiso 1 1 calc R . . . .
C17 C 0.4607(2) 0.2551(2) 0.81037(15) 0.0299(6) Uani 1 1 d . . . . .
C13 C 0.8495(3) 0.4401(2) 0.62050(15) 0.0321(6) Uani 1 1 d . . . . .
C21 C 0.6569(3) 0.1147(2) 0.84665(16) 0.0346(7) Uani 1 1 d . . . . .
C4 C 0.6196(3) 0.0654(2) 0.54712(15) 0.0343(7) Uani 1 1 d . . . . .
H4 H 0.598393 0.023800 0.510815 0.041 Uiso 1 1 calc R . . . .
C20 C 0.3583(3) 0.1905(2) 0.81786(19) 0.0405(7) Uani 1 1 d . . . . .
H20A H 0.339385 0.157193 0.774977 0.061 Uiso 1 1 calc GR . . . .
H20B H 0.291998 0.227183 0.828824 0.061 Uiso 1 1 calc GR . . . .
H20C H 0.378112 0.145971 0.854555 0.061 Uiso 1 1 calc GR . . . .
C8 C 0.7599(3) 0.5207(2) 0.87203(17) 0.0421(8) Uani 1 1 d . . . . .
H8A H 0.786690 0.579123 0.853801 0.063 Uiso 1 1 calc GR . . . .
H8B H 0.823287 0.490385 0.899245 0.063 Uiso 1 1 calc GR . . . .
H8C H 0.697575 0.533187 0.900825 0.063 Uiso 1 1 calc GR . . . .
C9 C 1.0076(3) 0.2879(3) 0.69032(18) 0.0440(8) Uani 1 1 d . . . . .
C16 C 0.9199(3) 0.4528(2) 0.55897(17) 0.0418(8) Uani 1 1 d . . . . .
H16A H 1.001714 0.453998 0.574600 0.063 Uiso 1 1 calc GR . . . .
H16B H 0.898414 0.511130 0.535961 0.063 Uiso 1 1 calc GR . . . .
H16C H 0.904584 0.401223 0.527118 0.063 Uiso 1 1 calc GR . . . .
C24 C 0.5724(3) 0.0520(2) 0.88003(19) 0.0490(9) Uani 1 1 d . . . . .
H24A H 0.527626 0.089047 0.909794 0.073 Uiso 1 1 calc GR . . . .
H24B H 0.614823 0.004174 0.907058 0.073 Uiso 1 1 calc GR . . . .
H24C H 0.520582 0.022551 0.844575 0.073 Uiso 1 1 calc GR . . . .
C10 C 1.0965(3) 0.2967(3) 0.6394(2) 0.0513(9) Uani 1 1 d . . . . .
H10A H 1.070265 0.263285 0.597539 0.077 Uiso 1 1 calc GR . . . .
H10B H 1.169215 0.270256 0.658830 0.077 Uiso 1 1 calc GR . . . .
H10C H 1.107467 0.362136 0.628752 0.077 Uiso 1 1 calc GR . . . .
C14 C 0.7222(3) 0.4523(3) 0.5979(2) 0.0498(9) Uani 1 1 d . . . . .
H14A H 0.697057 0.403212 0.565677 0.075 Uiso 1 1 calc GR . . . .
H14B H 0.709863 0.512695 0.575841 0.075 Uiso 1 1 calc GR . . . .
H14C H 0.677950 0.448897 0.637816 0.075 Uiso 1 1 calc GR . . . .
C19 C 0.4940(3) 0.3056(2) 0.87784(19) 0.0477(9) Uani 1 1 d . . . . .
H19A H 0.510440 0.260151 0.914328 0.071 Uiso 1 1 calc GR . . . .
H19B H 0.430602 0.345448 0.888946 0.071 Uiso 1 1 calc GR . . . .
H19C H 0.562292 0.343511 0.873300 0.071 Uiso 1 1 calc GR . . . .
C22 C 0.7363(3) 0.0529(3) 0.8084(2) 0.0561(10) Uani 1 1 d . . . . .
H22A H 0.690510 0.016715 0.773790 0.084 Uiso 1 1 calc GR . . . .
H22B H 0.778404 0.010906 0.840695 0.084 Uiso 1 1 calc GR . . . .
H22C H 0.790767 0.091644 0.786223 0.084 Uiso 1 1 calc GR . . . .
C18 C 0.4257(3) 0.3264(3) 0.7552(2) 0.0511(9) Uani 1 1 d . . . . .
H18A H 0.489857 0.368549 0.750041 0.077 Uiso 1 1 calc GR . . . .
H18B H 0.359683 0.361709 0.768204 0.077 Uiso 1 1 calc GR . . . .
H18C H 0.405081 0.294613 0.711832 0.077 Uiso 1 1 calc GR . . . .
C15 C 0.8853(4) 0.5145(3) 0.6735(2) 0.0613(12) Uani 1 1 d . . . . .
H15A H 0.841335 0.506830 0.713238 0.092 Uiso 1 1 calc GR . . . .
H15B H 0.870071 0.575880 0.653562 0.092 Uiso 1 1 calc GR . . . .
H15C H 0.967241 0.508479 0.687734 0.092 Uiso 1 1 calc GR . . . .
C23 C 0.7309(4) 0.1691(3) 0.9007(2) 0.0617(12) Uani 1 1 d . . . . .
H23A H 0.785058 0.207984 0.878403 0.093 Uiso 1 1 calc GR . . . .
H23B H 0.773386 0.125877 0.931865 0.093 Uiso 1 1 calc GR . . . .
H23C H 0.681743 0.208249 0.926357 0.093 Uiso 1 1 calc GR . . . .
C25 C 1.0432(4) 0.1394(4) 0.4518(2) 0.0694(13) Uani 1 1 d . . . . .
N4 N 0.9653(4) 0.1768(4) 0.4661(2) 0.0928(15) Uani 1 1 d . . . . .
C27 C 0.3433(5) 0.3015(4) 0.5239(2) 0.0746(14) Uani 1 1 d . . . . .
C12 C 1.0461(4) 0.3450(6) 0.7538(3) 0.115(3) Uani 1 1 d . . . . .
H12A H 1.045367 0.410850 0.742019 0.173 Uiso 1 1 calc GR . . . .
H12B H 1.123908 0.326633 0.771047 0.173 Uiso 1 1 calc GR . . . .
H12C H 0.993707 0.333945 0.789086 0.173 Uiso 1 1 calc GR . . . .
C28 C 0.4535(5) 0.2946(4) 0.5578(3) 0.0863(17) Uani 1 1 d . . . . .
H28A H 0.500747 0.346211 0.544168 0.129 Uiso 1 1 calc GR . . . .
H28B H 0.488573 0.235968 0.545896 0.129 Uiso 1 1 calc GR . . . .
H28C H 0.448234 0.297016 0.607197 0.129 Uiso 1 1 calc GR . . . .
N5 N 0.2561(5) 0.3130(6) 0.4952(3) 0.140(3) Uani 1 1 d . . . . .
C11 C 0.9990(4) 0.1860(4) 0.7082(3) 0.106(3) Uani 1 1 d . . . . .
H11A H 0.952218 0.178979 0.746757 0.160 Uiso 1 1 calc GR . . . .
H11B H 1.075914 0.161239 0.720739 0.160 Uiso 1 1 calc GR . . . .
H11C H 0.963381 0.152049 0.668804 0.160 Uiso 1 1 calc GR . . . .
C26 C 1.1463(6) 0.0933(5) 0.4329(3) 0.123(3) Uani 1 1 d . . . . .
H26A H 1.168921 0.119928 0.390299 0.184 Uiso 1 1 calc GR . . . .
H26B H 1.131067 0.027098 0.426487 0.184 Uiso 1 1 calc GR . . . .
H26C H 1.208382 0.102004 0.469103 0.184 Uiso 1 1 calc GR . . . .
H3 H 0.812(3) 0.365(2) 0.8381(16) 0.027(8) Uiso 1 1 d . . . . .
H1 H 0.485(3) 0.097(2) 0.7197(17) 0.032(10) Uiso 1 1 d . . . . .
H2 H 0.863(3) 0.250(2) 0.5585(17) 0.026(8) Uiso 1 1 d . . . . .


_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 P1 2.3003(7) . ?
Pd1 P2 2.3064(7) . ?
Pd1 N3 2.110(2) . ?
Pd1 C1 2.013(3) . ?
P1 N1 1.679(2) . ?
P1 C17 1.863(3) . ?
P1 C21 1.872(3) . ?
P2 N2 1.685(2) . ?
P2 C13 1.862(3) . ?
P2 C9 1.867(3) . ?
O1 C7 1.256(3) . ?
N3 C7 1.303(4) . ?
N1 C6 1.397(4) . ?
N2 C2 1.395(4) . ?
C1 C6 1.407(4) . ?
C1 C2 1.404(4) . ?
C6 C5 1.398(4) . ?
C2 C3 1.397(4) . ?
C7 C8 1.523(4) . ?
C3 C4 1.381(4) . ?
C5 C4 1.388(4) . ?
C17 C20 1.538(4) . ?
C17 C19 1.536(4) . ?
C17 C18 1.527(4) . ?
C13 C16 1.536(4) . ?
C13 C14 1.529(5) . ?
C13 C15 1.532(4) . ?
C21 C24 1.534(4) . ?
C21 C22 1.535(5) . ?
C21 C23 1.529(5) . ?
C9 C10 1.514(5) . ?
C9 C12 1.532(6) . ?
C9 C11 1.520(6) . ?
C25 N4 1.118(6) . ?
C25 C26 1.457(7) . ?
C27 C28 1.404(7) . ?
C27 N5 1.135(7) . ?

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
P1 Pd1 P2 161.42(3) . . ?
N3 Pd1 P1 98.74(7) . . ?
N3 Pd1 P2 98.79(7) . . ?
C1 Pd1 P1 81.11(8) . . ?
C1 Pd1 P2 81.49(8) . . ?
C1 Pd1 N3 178.75(10) . . ?
N1 P1 Pd1 102.71(9) . . ?
N1 P1 C17 104.10(14) . . ?
N1 P1 C21 105.71(14) . . ?
C17 P1 Pd1 119.22(9) . . ?
C17 P1 C21 112.29(14) . . ?
C21 P1 Pd1 111.13(10) . . ?
N2 P2 Pd1 102.19(9) . . ?
N2 P2 C13 103.18(14) . . ?
N2 P2 C9 104.93(15) . . ?
C13 P2 Pd1 117.68(10) . . ?
C13 P2 C9 113.30(16) . . ?
C9 P2 Pd1 113.37(12) . . ?
C7 N3 Pd1 125.8(2) . . ?
C6 N1 P1 116.2(2) . . ?
C2 N2 P2 117.5(2) . . ?
C6 C1 Pd1 121.1(2) . . ?
C2 C1 Pd1 121.4(2) . . ?
C2 C1 C6 117.5(2) . . ?
N1 C6 C1 117.7(2) . . ?
N1 C6 C5 121.1(3) . . ?
C5 C6 C1 121.2(3) . . ?
N2 C2 C1 117.3(2) . . ?
N2 C2 C3 121.0(3) . . ?
C3 C2 C1 121.7(3) . . ?
O1 C7 N3 123.4(3) . . ?
O1 C7 C8 117.8(3) . . ?
N3 C7 C8 118.8(3) . . ?
C4 C3 C2 119.0(3) . . ?
C4 C5 C6 119.2(3) . . ?
C20 C17 P1 113.5(2) . . ?
C19 C17 P1 110.2(2) . . ?
C19 C17 C20 110.2(3) . . ?
C18 C17 P1 105.2(2) . . ?
C18 C17 C20 108.4(3) . . ?
C18 C17 C19 109.0(3) . . ?
C16 C13 P2 113.8(2) . . ?
C14 C13 P2 104.1(2) . . ?
C14 C13 C16 109.6(3) . . ?
C14 C13 C15 108.5(3) . . ?
C15 C13 P2 111.9(2) . . ?
C15 C13 C16 108.7(3) . . ?
C24 C21 P1 114.1(2) . . ?
C24 C21 C22 108.0(3) . . ?
C22 C21 P1 105.3(2) . . ?
C23 C21 P1 110.4(2) . . ?
C23 C21 C24 110.7(3) . . ?
C23 C21 C22 108.0(3) . . ?
C3 C4 C5 121.4(3) . . ?
C10 C9 P2 115.3(3) . . ?
C10 C9 C12 109.0(4) . . ?
C10 C9 C11 107.4(3) . . ?
C12 C9 P2 109.7(3) . . ?
C11 C9 P2 104.7(3) . . ?
C11 C9 C12 110.7(5) . . ?
N4 C25 C26 178.3(7) . . ?
N5 C27 C28 175.3(8) . . ?

_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 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.741
####################################################################### 
# 
# 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_cjr-20211207
_database_code_depnum_ccdc_archive 'CCDC 2191733'
loop_
_audit_author_name
_audit_author_address
'Jie Zhang'
;Henan Normal University
China
;
_audit_update_record             
;
2022-10-25 deposited with the CCDC.	2022-11-02 downloaded from the CCDC.
;
_audit_creation_date             2022-10-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        tBu-PNCNP-Pd-NO3
_chemical_formula_moiety         'C22 H41 N3 O3 P2 Pd, C4 H8 O'
_chemical_formula_sum            'C26 H49 N3 O4 P2 Pd'
_chemical_formula_weight         636.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 N1 P1 N1 O1 Pd1'
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'
P P 0.2955 0.4335 '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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.34860(10)
_cell_length_b                   22.9353(2)
_cell_length_c                   11.59380(10)
_cell_angle_alpha                90
_cell_angle_beta                 95.3590(10)
_cell_angle_gamma                90
_cell_volume                     3004.48(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8916
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.4050
_cell_measurement_theta_min      3.8560
_shelx_estimated_absorpt_T_max   0.885
_shelx_estimated_absorpt_T_min   0.885
_exptl_absorpt_coefficient_mu    6.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.469
_diffrn_reflns_theta_min         3.855
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00 -20.00   1.00    1.00    --  -35.62 -60.00-151.00   83
  2  ω     -4.00  24.00   1.00    1.00    --  -35.62  60.00 -11.00   28
  3  ω     19.00  50.00   1.00    1.00    --   35.62  60.00 -11.00   31
  4  ω    -13.00  12.00   1.00    1.00    --   35.62 -60.00-151.00   25
  5  ω     58.00 124.00   1.00    1.93    --  107.12 -60.00-151.00   66
  6  ω    124.00 174.00   1.00    1.93    --  107.12  60.00 -11.00   50
  7  ω    -68.00 -42.00   1.00    1.00    --  -35.62-178.00   0.00   26
  8  ω     24.00  74.00   1.00    1.00    --   35.62 -99.00-120.00   50
  9  ω     63.00 104.00   1.00    1.00    --   35.62 178.00-120.00   41
 10  ω      2.00  70.00   1.00    1.00    --   35.62 -99.00  30.00   68
 11  ω     68.00 103.00   1.00    1.00    --   35.62  60.00 -11.00   35
 12  ω     81.00 109.00   1.00    1.93    --  107.12 -95.00 150.00   28
 13  ω     39.00 110.00   1.00    1.93    --  107.12 -95.00  90.00   71
 14  ω    117.00 176.00   1.00    1.93    --  107.12  30.00 -90.00   59
 15  ω     92.00 142.00   1.00    1.93    --  107.12 -15.00 -90.00   50
 16  ω     37.00  78.00   1.00    1.93    --  107.12 -15.00 -90.00   41
 17  ω     87.00 169.00   1.00    1.93    --  107.12  77.00 -60.00   82
 18  ω     58.00  91.00   1.00    1.93    --  107.12 -95.00 -30.00   33
 19  ω     38.00 105.00   1.00    1.93    --  107.12 -95.00-120.00   67
 20  ω    118.00 170.00   1.00    1.93    --  107.12 111.00 -90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0121725000
_diffrn_orient_matrix_UB_12      0.0070619000
_diffrn_orient_matrix_UB_13      0.1305026000
_diffrn_orient_matrix_UB_21      -0.0976680000
_diffrn_orient_matrix_UB_22      -0.0468587000
_diffrn_orient_matrix_UB_23      -0.0076617000
_diffrn_orient_matrix_UB_31      0.0943538000
_diffrn_orient_matrix_UB_32      -0.0476018000
_diffrn_orient_matrix_UB_33      0.0268931000
_diffrn_oxdiff_digest_frames     
;
01c353fbbfe26f25ed72ab21f8f48b06f6000303e19
;
_diffrn_oxdiff_digest_hkl        
;
0157bbce5127d6ee024c6fbd88ab43181e58f0
;
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5270
_reflns_number_total             5747
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.739
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0339
_refine_ls_restrained_S_all      1.037
_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)+(0.0531P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0878
_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:
 C25(H25A,H25B), C23(H23A,H23B), C26(H26A,H26B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C12(H12A,H12B,
 H12C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.63393(2) 0.35650(2) 0.41653(2) 0.00767(7) Uani 1 1 d . . . . .
P2 P 0.63353(5) 0.27637(3) 0.53997(5) 0.00945(13) Uani 1 1 d . . . . .
P1 P 0.69287(5) 0.42737(3) 0.29273(5) 0.00956(14) Uani 1 1 d . . . . .
O1 O 0.44905(16) 0.37648(9) 0.38994(16) 0.0152(4) Uani 1 1 d . . . . .
O4 O 0.99368(17) 0.50635(9) 0.21347(18) 0.0226(4) Uani 1 1 d . . . . .
O3 O 0.41424(18) 0.30362(10) 0.2710(2) 0.0282(5) Uani 1 1 d . . . . .
N2 N 0.7735(2) 0.27834(10) 0.6013(2) 0.0143(5) Uani 1 1 d . . . . .
N1 N 0.84070(19) 0.42136(10) 0.31191(19) 0.0135(4) Uani 1 1 d . . . . .
O2 O 0.27019(19) 0.35521(11) 0.3274(2) 0.0340(6) Uani 1 1 d . . . . .
C1 C 0.8082(2) 0.35006(11) 0.4576(2) 0.0092(5) Uani 1 1 d . . . . .
N3 N 0.3758(2) 0.34435(11) 0.3281(2) 0.0170(5) Uani 1 1 d . . . . .
C2 C 0.8543(2) 0.31189(12) 0.5448(2) 0.0111(5) Uani 1 1 d . . . . .
C6 C 0.8872(2) 0.38447(11) 0.4010(2) 0.0100(5) Uani 1 1 d . . . . .
C5 C 1.0092(2) 0.38109(12) 0.4312(2) 0.0129(5) Uani 1 1 d . . . . .
H5 H 1.062066 0.405114 0.393650 0.015 Uiso 1 1 calc R . . . .
C22 C 0.5251(2) 0.51125(13) 0.3389(3) 0.0233(6) Uani 1 1 d . . . . .
H22A H 0.482165 0.509429 0.261554 0.035 Uiso 1 1 calc GR . . . .
H22B H 0.509944 0.548893 0.374663 0.035 Uiso 1 1 calc GR . . . .
H22C H 0.498009 0.479693 0.386915 0.035 Uiso 1 1 calc GR . . . .
C11 C 0.5376(2) 0.28040(12) 0.6619(2) 0.0159(5) Uani 1 1 d . . . . .
C19 C 0.6585(2) 0.50455(12) 0.3286(2) 0.0150(5) Uani 1 1 d . . . . .
C4 C 1.0522(2) 0.34209(13) 0.5170(2) 0.0157(5) Uani 1 1 d . . . . .
H4 H 1.135149 0.339241 0.536955 0.019 Uiso 1 1 calc R . . . .
C13 C 0.4101(2) 0.29477(14) 0.6124(3) 0.0225(6) Uani 1 1 d . . . . .
H13A H 0.409435 0.332026 0.571015 0.034 Uiso 1 1 calc GR . . . .
H13B H 0.359199 0.297544 0.675982 0.034 Uiso 1 1 calc GR . . . .
H13C H 0.380732 0.263866 0.558895 0.034 Uiso 1 1 calc GR . . . .
C3 C 0.9762(2) 0.30735(12) 0.5739(2) 0.0149(5) Uani 1 1 d . . . . .
H3 H 1.006634 0.280748 0.632021 0.018 Uiso 1 1 calc R . . . .
C20 C 0.6991(3) 0.54990(13) 0.2431(3) 0.0243(6) Uani 1 1 d . . . . .
H20A H 0.782386 0.543064 0.231232 0.036 Uiso 1 1 calc GR . . . .
H20B H 0.690247 0.589133 0.274618 0.036 Uiso 1 1 calc GR . . . .
H20C H 0.650663 0.546419 0.168895 0.036 Uiso 1 1 calc GR . . . .
C12 C 0.5375(3) 0.22562(14) 0.7377(3) 0.0240(6) Uani 1 1 d . . . . .
H12A H 0.501842 0.193174 0.691821 0.036 Uiso 1 1 calc GR . . . .
H12B H 0.491592 0.233072 0.803684 0.036 Uiso 1 1 calc GR . . . .
H12C H 0.619055 0.215614 0.766049 0.036 Uiso 1 1 calc GR . . . .
C15 C 0.6552(3) 0.40974(13) 0.1363(2) 0.0185(6) Uani 1 1 d . . . . .
C17 C 0.6717(3) 0.34347(15) 0.1274(3) 0.0282(7) Uani 1 1 d . . . . .
H17A H 0.752065 0.332963 0.158773 0.042 Uiso 1 1 calc GR . . . .
H17B H 0.659273 0.331544 0.046043 0.042 Uiso 1 1 calc GR . . . .
H17C H 0.614198 0.323622 0.171837 0.042 Uiso 1 1 calc GR . . . .
C7 C 0.6221(2) 0.20385(12) 0.4642(2) 0.0171(6) Uani 1 1 d . . . . .
C14 C 0.5857(3) 0.33147(14) 0.7380(3) 0.0254(7) Uani 1 1 d . . . . .
H14A H 0.663536 0.321139 0.776332 0.038 Uiso 1 1 calc GR . . . .
H14B H 0.531173 0.339787 0.796666 0.038 Uiso 1 1 calc GR . . . .
H14C H 0.593121 0.366063 0.689607 0.038 Uiso 1 1 calc GR . . . .
C8 C 0.6817(3) 0.21251(13) 0.3518(2) 0.0220(6) Uani 1 1 d . . . . .
H8A H 0.637421 0.241511 0.303157 0.033 Uiso 1 1 calc GR . . . .
H8B H 0.682642 0.175401 0.310004 0.033 Uiso 1 1 calc GR . . . .
H8C H 0.763086 0.226137 0.370586 0.033 Uiso 1 1 calc GR . . . .
C10 C 0.6911(3) 0.15616(13) 0.5352(3) 0.0272(7) Uani 1 1 d . . . . .
H10A H 0.775207 0.166469 0.545255 0.041 Uiso 1 1 calc GR . . . .
H10B H 0.681270 0.118829 0.494356 0.041 Uiso 1 1 calc GR . . . .
H10C H 0.660658 0.152815 0.611340 0.041 Uiso 1 1 calc GR . . . .
C21 C 0.7245(3) 0.51534(14) 0.4487(3) 0.0239(6) Uani 1 1 d . . . . .
H21A H 0.703266 0.484944 0.502473 0.036 Uiso 1 1 calc GR . . . .
H21B H 0.702248 0.553580 0.477554 0.036 Uiso 1 1 calc GR . . . .
H21C H 0.810052 0.514369 0.442708 0.036 Uiso 1 1 calc GR . . . .
C25 C 1.2014(3) 0.49431(16) 0.2222(3) 0.0276(7) Uani 1 1 d . . . . .
H25A H 1.264450 0.495579 0.168719 0.033 Uiso 1 1 calc R . . . .
H25B H 1.226053 0.467931 0.287615 0.033 Uiso 1 1 calc R . . . .
C16 C 0.7375(3) 0.43957(16) 0.0566(3) 0.0324(8) Uani 1 1 d . . . . .
H16A H 0.728054 0.481951 0.061136 0.049 Uiso 1 1 calc GR . . . .
H16B H 0.717310 0.426667 -0.023410 0.049 Uiso 1 1 calc GR . . . .
H16C H 0.819819 0.429124 0.081088 0.049 Uiso 1 1 calc GR . . . .
C18 C 0.5257(3) 0.42504(16) 0.0980(3) 0.0293(7) Uani 1 1 d . . . . .
H18A H 0.474374 0.408373 0.152990 0.044 Uiso 1 1 calc GR . . . .
H18B H 0.503719 0.409000 0.020640 0.044 Uiso 1 1 calc GR . . . .
H18C H 0.516237 0.467514 0.095982 0.044 Uiso 1 1 calc GR . . . .
C23 C 1.0485(3) 0.54671(14) 0.2968(3) 0.0282(7) Uani 1 1 d . . . . .
H23A H 1.048966 0.530779 0.376182 0.034 Uiso 1 1 calc R . . . .
H23B H 1.005519 0.584315 0.293118 0.034 Uiso 1 1 calc R . . . .
C26 C 1.0845(3) 0.47543(15) 0.1600(3) 0.0266(7) Uani 1 1 d . . . . .
H26A H 1.081520 0.485231 0.076601 0.032 Uiso 1 1 calc R . . . .
H26B H 1.073781 0.432819 0.167720 0.032 Uiso 1 1 calc R . . . .
C24 C 1.1732(3) 0.55487(15) 0.2647(3) 0.0298(7) Uani 1 1 d . . . . .
H24A H 1.227598 0.566294 0.332736 0.036 Uiso 1 1 calc R . . . .
H24B H 1.176797 0.584402 0.202896 0.036 Uiso 1 1 calc R . . . .
C9 C 0.4933(3) 0.18464(15) 0.4332(3) 0.0293(7) Uani 1 1 d . . . . .
H9A H 0.457368 0.174500 0.504174 0.044 Uiso 1 1 calc GR . . . .
H9B H 0.491775 0.150575 0.382064 0.044 Uiso 1 1 calc GR . . . .
H9C H 0.448758 0.216592 0.393618 0.044 Uiso 1 1 calc GR . . . .
H2 H 0.803(3) 0.2579(15) 0.646(3) 0.015(8) Uiso 1 1 d . . . . .
H1 H 0.883(3) 0.4446(15) 0.282(3) 0.020(9) Uiso 1 1 d . . . . .


_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 P2 2.3296(6) . ?
Pd1 P1 2.3084(6) . ?
Pd1 O1 2.1415(18) . ?
Pd1 C1 1.996(3) . ?
P2 N2 1.679(2) . ?
P2 C11 1.866(3) . ?
P2 C7 1.880(3) . ?
P1 N1 1.677(2) . ?
P1 C19 1.868(3) . ?
P1 C15 1.868(3) . ?
O1 N3 1.279(3) . ?
O4 C23 1.437(4) . ?
O4 C26 1.438(4) . ?
O3 N3 1.247(3) . ?
N2 C2 1.405(3) . ?
N2 H2 0.75(3) . ?
N1 C6 1.400(3) . ?
N1 H1 0.82(4) . ?
O2 N3 1.224(3) . ?
C1 C2 1.401(4) . ?
C1 C6 1.403(4) . ?
C2 C3 1.397(3) . ?
C6 C5 1.398(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.392(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 C19 1.538(4) . ?
C11 C13 1.540(4) . ?
C11 C12 1.533(4) . ?
C11 C14 1.536(4) . ?
C19 C20 1.537(4) . ?
C19 C21 1.539(4) . ?
C4 H4 0.9500 . ?
C4 C3 1.386(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C3 H3 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C15 C17 1.536(4) . ?
C15 C16 1.535(4) . ?
C15 C18 1.536(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C7 C8 1.536(4) . ?
C7 C10 1.538(4) . ?
C7 C9 1.536(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.513(4) . ?
C25 C24 1.518(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.508(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
P1 Pd1 P2 162.70(2) . . ?
O1 Pd1 P2 101.49(6) . . ?
O1 Pd1 P1 95.55(6) . . ?
C1 Pd1 P2 81.59(8) . . ?
C1 Pd1 P1 82.08(8) . . ?
C1 Pd1 O1 170.32(9) . . ?
N2 P2 Pd1 100.53(8) . . ?
N2 P2 C11 105.91(12) . . ?
N2 P2 C7 104.05(12) . . ?
C11 P2 Pd1 117.46(9) . . ?
C11 P2 C7 112.22(13) . . ?
C7 P2 Pd1 114.52(9) . . ?
N1 P1 Pd1 101.77(8) . . ?
N1 P1 C19 105.98(12) . . ?
N1 P1 C15 104.25(12) . . ?
C19 P1 Pd1 116.77(9) . . ?
C19 P1 C15 112.80(13) . . ?
C15 P1 Pd1 113.44(9) . . ?
N3 O1 Pd1 122.26(17) . . ?
C23 O4 C26 108.9(2) . . ?
P2 N2 H2 128(3) . . ?
C2 N2 P2 116.77(18) . . ?
C2 N2 H2 113(3) . . ?
P1 N1 H1 121(2) . . ?
C6 N1 P1 116.82(18) . . ?
C6 N1 H1 121(2) . . ?
C2 C1 Pd1 120.88(19) . . ?
C2 C1 C6 118.5(2) . . ?
C6 C1 Pd1 120.62(19) . . ?
O3 N3 O1 119.2(2) . . ?
O2 N3 O1 118.1(2) . . ?
O2 N3 O3 122.7(2) . . ?
C1 C2 N2 117.5(2) . . ?
C3 C2 N2 121.4(2) . . ?
C3 C2 C1 121.0(2) . . ?
N1 C6 C1 118.1(2) . . ?
C5 C6 N1 121.0(2) . . ?
C5 C6 C1 120.9(2) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 C6 119.2(2) . . ?
C4 C5 H5 120.4 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
C13 C11 P2 108.83(18) . . ?
C12 C11 P2 115.2(2) . . ?
C12 C11 C13 109.8(2) . . ?
C12 C11 C14 108.3(2) . . ?
C14 C11 P2 105.76(19) . . ?
C14 C11 C13 108.8(2) . . ?
C22 C19 P1 109.84(19) . . ?
C22 C19 C21 108.3(2) . . ?
C20 C19 P1 114.6(2) . . ?
C20 C19 C22 109.8(2) . . ?
C20 C19 C21 109.0(2) . . ?
C21 C19 P1 105.05(19) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 C5 121.1(2) . . ?
C3 C4 H4 119.4 . . ?
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 . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.3(2) . . ?
C4 C3 H3 120.4 . . ?
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 . . ?
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 . . ?
C17 C15 P1 105.13(19) . . ?
C17 C15 C18 109.0(3) . . ?
C16 C15 P1 113.0(2) . . ?
C16 C15 C17 108.4(3) . . ?
C16 C15 C18 110.1(3) . . ?
C18 C15 P1 110.9(2) . . ?
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 . . ?
C8 C7 P2 105.39(19) . . ?
C8 C7 C10 107.7(2) . . ?
C8 C7 C9 108.8(2) . . ?
C10 C7 P2 111.7(2) . . ?
C9 C7 P2 112.7(2) . . ?
C9 C7 C10 110.3(3) . . ?
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 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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 . . ?
H25A C25 H25B 109.2 . . ?
C26 C25 H25A 111.3 . . ?
C26 C25 H25B 111.3 . . ?
C26 C25 C24 102.4(3) . . ?
C24 C25 H25A 111.3 . . ?
C24 C25 H25B 111.3 . . ?
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 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 . . ?
O4 C23 H23A 110.6 . . ?
O4 C23 H23B 110.6 . . ?
O4 C23 C24 105.8(2) . . ?
H23A C23 H23B 108.7 . . ?
C24 C23 H23A 110.6 . . ?
C24 C23 H23B 110.6 . . ?
O4 C26 C25 106.6(3) . . ?
O4 C26 H26A 110.4 . . ?
O4 C26 H26B 110.4 . . ?
C25 C26 H26A 110.4 . . ?
C25 C26 H26B 110.4 . . ?
H26A C26 H26B 108.6 . . ?
C25 C24 H24A 111.5 . . ?
C25 C24 H24B 111.5 . . ?
C23 C24 C25 101.4(3) . . ?
C23 C24 H24A 111.5 . . ?
C23 C24 H24B 111.5 . . ?
H24A C24 H24B 109.3 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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 P2 N2 C2 -17.0(2) . . . . ?
Pd1 P2 C11 C13 54.3(2) . . . . ?
Pd1 P2 C11 C12 177.95(18) . . . . ?
Pd1 P2 C11 C14 -62.5(2) . . . . ?
Pd1 P2 C7 C8 30.0(2) . . . . ?
Pd1 P2 C7 C10 146.66(19) . . . . ?
Pd1 P2 C7 C9 -88.6(2) . . . . ?
Pd1 P1 N1 C6 -8.0(2) . . . . ?
Pd1 P1 C19 C22 -55.5(2) . . . . ?
Pd1 P1 C19 C20 -179.72(17) . . . . ?
Pd1 P1 C19 C21 60.7(2) . . . . ?
Pd1 P1 C15 C17 -36.2(2) . . . . ?
Pd1 P1 C15 C16 -154.3(2) . . . . ?
Pd1 P1 C15 C18 81.5(2) . . . . ?
Pd1 O1 N3 O3 -8.0(3) . . . . ?
Pd1 O1 N3 O2 172.2(2) . . . . ?
Pd1 C1 C2 N2 0.3(3) . . . . ?
Pd1 C1 C2 C3 -179.88(19) . . . . ?
Pd1 C1 C6 N1 -2.7(3) . . . . ?
Pd1 C1 C6 C5 178.56(19) . . . . ?
P2 N2 C2 C1 13.0(3) . . . . ?
P2 N2 C2 C3 -166.8(2) . . . . ?
P1 N1 C6 C1 7.7(3) . . . . ?
P1 N1 C6 C5 -173.56(19) . . . . ?
O4 C23 C24 C25 -35.2(3) . . . . ?
N2 P2 C11 C13 165.5(2) . . . . ?
N2 P2 C11 C12 -70.8(2) . . . . ?
N2 P2 C11 C14 48.8(2) . . . . ?
N2 P2 C7 C8 -78.7(2) . . . . ?
N2 P2 C7 C10 37.9(2) . . . . ?
N2 P2 C7 C9 162.7(2) . . . . ?
N2 C2 C3 C4 -178.9(3) . . . . ?
N1 P1 C19 C22 -167.99(19) . . . . ?
N1 P1 C19 C20 67.8(2) . . . . ?
N1 P1 C19 C21 -51.8(2) . . . . ?
N1 P1 C15 C17 73.7(2) . . . . ?
N1 P1 C15 C16 -44.4(3) . . . . ?
N1 P1 C15 C18 -168.6(2) . . . . ?
N1 C6 C5 C4 -177.3(2) . . . . ?
C1 C2 C3 C4 1.3(4) . . . . ?
C1 C6 C5 C4 1.3(4) . . . . ?
C2 C1 C6 N1 178.3(2) . . . . ?
C2 C1 C6 C5 -0.4(4) . . . . ?
C6 C1 C2 N2 179.3(2) . . . . ?
C6 C1 C2 C3 -0.9(4) . . . . ?
C6 C5 C4 C3 -1.0(4) . . . . ?
C5 C4 C3 C2 -0.3(4) . . . . ?
C11 P2 N2 C2 -139.7(2) . . . . ?
C11 P2 C7 C8 167.23(18) . . . . ?
C11 P2 C7 C10 -76.1(2) . . . . ?
C11 P2 C7 C9 48.7(2) . . . . ?
C19 P1 N1 C6 114.6(2) . . . . ?
C19 P1 C15 C17 -171.82(19) . . . . ?
C19 P1 C15 C16 70.1(3) . . . . ?
C19 P1 C15 C18 -54.1(2) . . . . ?
C15 P1 N1 C6 -126.2(2) . . . . ?
C15 P1 C19 C22 78.5(2) . . . . ?
C15 P1 C19 C20 -45.7(2) . . . . ?
C15 P1 C19 C21 -165.23(19) . . . . ?
C7 P2 N2 C2 101.8(2) . . . . ?
C7 P2 C11 C13 -81.6(2) . . . . ?
C7 P2 C11 C12 42.1(2) . . . . ?
C7 P2 C11 C14 161.69(19) . . . . ?
C23 O4 C26 C25 5.3(3) . . . . ?
C26 O4 C23 C24 19.1(3) . . . . ?
C26 C25 C24 C23 37.3(3) . . . . ?
C24 C25 C26 O4 -27.1(3) . . . . ?

_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 1.946
_oxdiff_exptl_absorpt_empirical_full_min 0.538
####################################################################### 
# 
# 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_20211007-cjr
_database_code_depnum_ccdc_archive 'CCDC 2191734'
loop_
_audit_author_name
_audit_author_address
'Jie Zhang'
;Henan Normal University
China
;
_audit_update_record             
;
2022-10-25 deposited with the CCDC.	2022-11-02 downloaded from the CCDC.
;
_audit_creation_date             2022-10-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        tBu-PNCNP-Pd0OH
_chemical_formula_moiety         'C22 H42 N2 O P2 Pd, 3(H2 O)'
_chemical_formula_sum            'C22 H48 N2 O4 P2 Pd'
_chemical_formula_weight         572.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 N1 P1 Pd1'
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'
P P 0.2955 0.4335 '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           61
_space_group_name_H-M_alt        'P b c a'
_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'
'-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                   16.9062(2)
_cell_length_b                   14.9710(2)
_cell_length_c                   21.5306(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5449.45(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7457
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.4490
_cell_measurement_theta_min      4.4310
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.923
_exptl_absorpt_coefficient_mu    6.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.011
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14725
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.455
_diffrn_reflns_theta_min         4.107
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00   7.00   1.00    1.22    --  -35.62  94.00 157.00   78
  2  ω      0.00  26.00   1.00    1.22    --   35.62 -95.00 -51.00   26
  3  ω    130.00 176.00   1.00    4.89    --  107.12  94.00 157.00   46
  4  ω     70.00 109.00   1.00    4.89    --  107.12 -95.00 -51.00   39
  5  ω     97.00 154.00   1.00    4.89    --  107.12  41.00 -50.00   57
  6  ω     63.00  90.00   1.00    4.89    --  107.12 -94.00  46.00   27
  7  ω    -74.00 -35.00   1.00    1.22    --  -35.62-178.00 150.00   39
  8  ω     70.00 100.00   1.00    1.22    --   35.62  77.00  90.00   30
  9  ω     63.00 107.00   1.00    1.22    --   35.62 178.00  90.00   44
 10  ω     64.00  89.00   1.00    1.22    --   35.62 178.00 -30.00   25
 11  ω     14.00  48.00   1.00    1.22    --   35.62  77.00  90.00   34
 12  ω     90.00 162.00   1.00    4.89    --  107.12  61.00  60.00   72
 13  ω    110.00 175.00   1.00    4.89    --  107.12 111.00 -60.00   65
 14  ω     71.00  97.00   1.00    4.89    --  107.12 -95.00-120.00   26
 15  ω     62.00  95.00   1.00    4.89    --  107.12 -95.00-150.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0280859000
_diffrn_orient_matrix_UB_12      -0.0198502000
_diffrn_orient_matrix_UB_13      -0.0666727000
_diffrn_orient_matrix_UB_21      0.0379185000
_diffrn_orient_matrix_UB_22      0.0934703000
_diffrn_orient_matrix_UB_23      -0.0036479000
_diffrn_orient_matrix_UB_31      0.0779153000
_diffrn_orient_matrix_UB_32      -0.0382740000
_diffrn_orient_matrix_UB_33      0.0257264000
_diffrn_oxdiff_digest_frames     
;
01ceeb07ab268c14b21fd3d029f13b2c83000361b0a
;
_diffrn_oxdiff_digest_hkl        
;
01500877d8d1519637b8f1df0095198fbc5f9c
;
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4653
_reflns_number_total             5210
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.073
_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     310
_refine_ls_number_reflns         5210
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.165
_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)+(0.0360P)²+3.7093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0785
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1-O2
 3.5 with sigma of 0.02
 H3B-H4A
 2.5 with sigma of 0.02
 H2B-H3B
 2.5 with sigma of 0.02
3.a Free rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B)
3.b Rotating group:
 O1(H1)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C),
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C14(H14A,H14B,
 H14C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.40786(2) 0.24256(2) 0.37171(2) 0.01568(7) Uani 1 1 d . . . . .
P2 P 0.31624(3) 0.18729(4) 0.44060(3) 0.01724(13) Uani 1 1 d . . . . .
P1 P 0.48642(4) 0.26226(4) 0.28551(3) 0.01719(13) Uani 1 1 d . . . . .
O1 O 0.45683(12) 0.34612(12) 0.42807(9) 0.0273(4) Uani 1 1 d D . . . .
H1 H 0.449386 0.335614 0.469990 0.041 Uiso 1 1 d GR . . . .
N2 N 0.26313(13) 0.11712(15) 0.39609(10) 0.0212(4) Uani 1 1 d . . . . .
N1 N 0.45333(13) 0.18215(15) 0.23722(11) 0.0229(5) Uani 1 1 d . . . . .
C1 C 0.35836(14) 0.14988(16) 0.31659(12) 0.0180(5) Uani 1 1 d . . . . .
C2 C 0.29290(14) 0.09955(16) 0.33669(12) 0.0191(5) Uani 1 1 d . . . . .
C6 C 0.38600(14) 0.13491(17) 0.25636(12) 0.0205(5) Uani 1 1 d . . . . .
C5 C 0.34841(15) 0.07454(18) 0.21629(13) 0.0245(5) Uani 1 1 d . . . . .
H5 H 0.366135 0.067501 0.174707 0.029 Uiso 1 1 calc R . . . .
C4 C 0.28467(15) 0.02509(17) 0.23847(13) 0.0248(5) Uani 1 1 d . . . . .
H4 H 0.259444 -0.016718 0.211832 0.030 Uiso 1 1 calc R . . . .
C11 C 0.59326(14) 0.23450(18) 0.29663(14) 0.0227(5) Uani 1 1 d . . . . .
C3 C 0.25741(14) 0.03569(17) 0.29852(13) 0.0225(5) Uani 1 1 d . . . . .
H3 H 0.215114 0.000011 0.313631 0.027 Uiso 1 1 calc R . . . .
C9 C 0.47401(17) 0.44653(17) 0.29193(13) 0.0263(6) Uani 1 1 d . . . . .
H9A H 0.433605 0.436662 0.323845 0.039 Uiso 1 1 calc GR . . . .
H9B H 0.464079 0.503617 0.271075 0.039 Uiso 1 1 calc GR . . . .
H9C H 0.526401 0.447826 0.311386 0.039 Uiso 1 1 calc GR . . . .
C7 C 0.47077(15) 0.37050(16) 0.24414(12) 0.0205(5) Uani 1 1 d . . . . .
C8 C 0.52840(16) 0.38921(19) 0.19066(13) 0.0274(6) Uani 1 1 d . . . . .
H8A H 0.581942 0.396743 0.207290 0.041 Uiso 1 1 calc GR . . . .
H8B H 0.512344 0.443874 0.169026 0.041 Uiso 1 1 calc GR . . . .
H8C H 0.527719 0.338956 0.161493 0.041 Uiso 1 1 calc GR . . . .
C15 C 0.24208(16) 0.26900(19) 0.47021(14) 0.0279(6) Uani 1 1 d . . . . .
C12 C 0.59350(17) 0.15058(19) 0.33812(15) 0.0311(6) Uani 1 1 d . . . . .
H12A H 0.570247 0.165092 0.378575 0.047 Uiso 1 1 calc GR . . . .
H12B H 0.648010 0.129958 0.343942 0.047 Uiso 1 1 calc GR . . . .
H12C H 0.562386 0.103343 0.318217 0.047 Uiso 1 1 calc GR . . . .
C19 C 0.36031(17) 0.11578(18) 0.50290(13) 0.0274(6) Uani 1 1 d . . . . .
C22 C 0.4239(2) 0.1681(2) 0.53809(15) 0.0401(8) Uani 1 1 d . . . . .
H22A H 0.463925 0.189537 0.508744 0.060 Uiso 1 1 calc GR . . . .
H22B H 0.448920 0.129103 0.568911 0.060 Uiso 1 1 calc GR . . . .
H22C H 0.399517 0.219201 0.559158 0.060 Uiso 1 1 calc GR . . . .
C10 C 0.38577(16) 0.3658(2) 0.21836(14) 0.0297(6) Uani 1 1 d . . . . .
H10A H 0.383182 0.320660 0.185459 0.045 Uiso 1 1 calc GR . . . .
H10B H 0.370865 0.424145 0.201375 0.045 Uiso 1 1 calc GR . . . .
H10C H 0.349260 0.349594 0.251870 0.045 Uiso 1 1 calc GR . . . .
C13 C 0.63500(16) 0.30999(19) 0.33080(15) 0.0310(6) Uani 1 1 d . . . . .
H13A H 0.634937 0.363742 0.304833 0.047 Uiso 1 1 calc GR . . . .
H13B H 0.689674 0.292440 0.339752 0.047 Uiso 1 1 calc GR . . . .
H13C H 0.607274 0.322375 0.369837 0.047 Uiso 1 1 calc GR . . . .
C17 C 0.16260(18) 0.2247(2) 0.48735(19) 0.0429(8) Uani 1 1 d . . . . .
H17A H 0.140580 0.194935 0.450679 0.064 Uiso 1 1 calc GR . . . .
H17B H 0.125533 0.270404 0.501975 0.064 Uiso 1 1 calc GR . . . .
H17C H 0.171220 0.180566 0.520292 0.064 Uiso 1 1 calc GR . . . .
C14 C 0.63561(18) 0.2132(2) 0.23565(15) 0.0364(7) Uani 1 1 d . . . . .
H14A H 0.606834 0.166057 0.213620 0.055 Uiso 1 1 calc GR . . . .
H14B H 0.689567 0.192986 0.244505 0.055 Uiso 1 1 calc GR . . . .
H14C H 0.637562 0.267010 0.209749 0.055 Uiso 1 1 calc GR . . . .
C21 C 0.40077(19) 0.0395(2) 0.46815(17) 0.0392(8) Uani 1 1 d . . . . .
H21A H 0.361477 0.006975 0.443503 0.059 Uiso 1 1 calc GR . . . .
H21B H 0.425312 -0.001272 0.498087 0.059 Uiso 1 1 calc GR . . . .
H21C H 0.441508 0.063904 0.440561 0.059 Uiso 1 1 calc GR . . . .
C16 C 0.2738(2) 0.3220(2) 0.52528(15) 0.0390(7) Uani 1 1 d . . . . .
H16A H 0.279718 0.282253 0.561145 0.059 Uiso 1 1 calc GR . . . .
H16B H 0.236656 0.370053 0.535569 0.059 Uiso 1 1 calc GR . . . .
H16C H 0.325267 0.347728 0.514533 0.059 Uiso 1 1 calc GR . . . .
C18 C 0.22780(19) 0.3319(2) 0.41513(16) 0.0385(7) Uani 1 1 d . . . . .
H18A H 0.274373 0.369888 0.409032 0.058 Uiso 1 1 calc GR . . . .
H18B H 0.181560 0.369455 0.423638 0.058 Uiso 1 1 calc GR . . . .
H18C H 0.218328 0.296621 0.377526 0.058 Uiso 1 1 calc GR . . . .
C20 C 0.2987(2) 0.0776(2) 0.54812(15) 0.0408(8) Uani 1 1 d . . . . .
H20A H 0.276138 0.126165 0.572940 0.061 Uiso 1 1 calc GR . . . .
H20B H 0.324154 0.034127 0.575679 0.061 Uiso 1 1 calc GR . . . .
H20C H 0.256536 0.048070 0.524575 0.061 Uiso 1 1 calc GR . . . .
O2 O 0.38034(13) 0.50932(14) 0.43769(10) 0.0315(4) Uani 1 1 d D . . . .
H2A H 0.395479 0.456390 0.429829 0.047 Uiso 1 1 d G . . . .
H2B H 0.390881 0.516526 0.475992 0.047 Uiso 1 1 d DG . . . .
O3 O 0.42305(15) 0.53375(18) 0.56101(12) 0.0450(6) Uani 1 1 d . . . . .
H3A H 0.463488 0.564697 0.570353 0.067 Uiso 1 1 d G . . . .
H3B H 0.415154 0.500926 0.592587 0.067 Uiso 1 1 d DG . . . .
O4 O 0.49937(17) 0.37161(17) 0.60527(13) 0.0491(6) Uani 1 1 d . . . . .
H4A H 0.486828 0.362775 0.567515 0.074 Uiso 1 1 d DG . . . .
H4B H 0.535170 0.411341 0.603782 0.074 Uiso 1 1 d G . . . .
H2 H 0.2264(19) 0.084(2) 0.4112(15) 0.025(8) Uiso 1 1 d . . . . .
H1A H 0.4701(18) 0.176(2) 0.2025(15) 0.019(7) Uiso 1 1 d . . . . .


_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 P2 2.2985(6) . ?
Pd1 P1 2.3012(6) . ?
Pd1 O1 2.1358(17) . ?
Pd1 C1 2.008(2) . ?
P2 N2 1.682(2) . ?
P2 C15 1.864(3) . ?
P2 C19 1.871(3) . ?
P1 N1 1.683(2) . ?
P1 C11 1.869(3) . ?
P1 C7 1.868(3) . ?
O1 H1 0.9248 . ?
N2 C2 1.399(3) . ?
N2 H2 0.86(3) . ?
N1 C6 1.402(3) . ?
N1 H1A 0.80(3) . ?
C1 C2 1.407(4) . ?
C1 C6 1.396(4) . ?
C2 C3 1.396(3) . ?
C6 C5 1.402(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.392(4) . ?
C4 H4 0.9500 . ?
C4 C3 1.382(4) . ?
C11 C12 1.542(4) . ?
C11 C13 1.522(4) . ?
C11 C14 1.529(4) . ?
C3 H3 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C7 1.535(3) . ?
C7 C8 1.534(4) . ?
C7 C10 1.542(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C15 C17 1.543(4) . ?
C15 C16 1.524(4) . ?
C15 C18 1.534(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C19 C22 1.531(4) . ?
C19 C21 1.527(4) . ?
C19 C20 1.536(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
O2 H2A 0.8498 . ?
O2 H2B 0.8505 . ?
O3 H3A 0.8500 . ?
O3 H3B 0.8494 . ?
O4 H4A 0.8503 . ?
O4 H4B 0.8493 . ?

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
P2 Pd1 P1 162.84(2) . . ?
O1 Pd1 P2 98.97(6) . . ?
O1 Pd1 P1 98.13(6) . . ?
C1 Pd1 P2 81.48(8) . . ?
C1 Pd1 P1 81.52(8) . . ?
C1 Pd1 O1 177.08(9) . . ?
N2 P2 Pd1 102.53(8) . . ?
N2 P2 C15 104.22(12) . . ?
N2 P2 C19 105.29(12) . . ?
C15 P2 Pd1 115.96(9) . . ?
C15 P2 C19 113.46(14) . . ?
C19 P2 Pd1 113.60(10) . . ?
N1 P1 Pd1 102.42(8) . . ?
N1 P1 C11 104.00(12) . . ?
N1 P1 C7 106.05(12) . . ?
C11 P1 Pd1 115.22(9) . . ?
C7 P1 Pd1 114.46(8) . . ?
C7 P1 C11 113.01(12) . . ?
Pd1 O1 H1 112.2 . . ?
P2 N2 H2 122(2) . . ?
C2 N2 P2 116.49(17) . . ?
C2 N2 H2 120(2) . . ?
P1 N1 H1A 122(2) . . ?
C6 N1 P1 116.59(18) . . ?
C6 N1 H1A 120(2) . . ?
C2 C1 Pd1 121.06(18) . . ?
C6 C1 Pd1 121.34(18) . . ?
C6 C1 C2 117.6(2) . . ?
N2 C2 C1 117.6(2) . . ?
C3 C2 N2 120.8(2) . . ?
C3 C2 C1 121.6(2) . . ?
C1 C6 N1 117.6(2) . . ?
C1 C6 C5 121.6(2) . . ?
C5 C6 N1 120.8(2) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 C6 118.9(3) . . ?
C4 C5 H5 120.6 . . ?
C5 C4 H4 119.4 . . ?
C3 C4 C5 121.2(2) . . ?
C3 C4 H4 119.4 . . ?
C12 C11 P1 104.95(18) . . ?
C13 C11 P1 110.18(18) . . ?
C13 C11 C12 108.9(2) . . ?
C13 C11 C14 110.7(2) . . ?
C14 C11 P1 112.9(2) . . ?
C14 C11 C12 109.1(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.1(2) . . ?
C4 C3 H3 120.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
C9 C7 P1 108.57(18) . . ?
C9 C7 C10 108.0(2) . . ?
C8 C7 P1 115.24(18) . . ?
C8 C7 C9 110.2(2) . . ?
C8 C7 C10 109.3(2) . . ?
C10 C7 P1 105.31(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C17 C15 P2 112.7(2) . . ?
C16 C15 P2 111.8(2) . . ?
C16 C15 C17 110.1(3) . . ?
C16 C15 C18 109.7(3) . . ?
C18 C15 P2 104.2(2) . . ?
C18 C15 C17 108.2(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 . . ?
C22 C19 P2 109.97(19) . . ?
C22 C19 C20 110.7(3) . . ?
C21 C19 P2 104.8(2) . . ?
C21 C19 C22 108.1(3) . . ?
C21 C19 C20 109.6(3) . . ?
C20 C19 P2 113.4(2) . . ?
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 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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 . . ?
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 . . ?
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 . . ?
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 . . ?
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 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 . . ?
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 . . ?
H2A O2 H2B 104.4 . . ?
H3A O3 H3B 104.6 . . ?
H4A O4 H4B 104.5 . . ?

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 P2 N2 C2 9.66(19) . . . . ?
Pd1 P2 C15 C17 151.2(2) . . . . ?
Pd1 P2 C15 C16 -84.2(2) . . . . ?
Pd1 P2 C15 C18 34.2(2) . . . . ?
Pd1 P2 C19 C22 56.6(2) . . . . ?
Pd1 P2 C19 C21 -59.4(2) . . . . ?
Pd1 P2 C19 C20 -178.93(19) . . . . ?
Pd1 P1 N1 C6 7.1(2) . . . . ?
Pd1 P1 C11 C12 38.9(2) . . . . ?
Pd1 P1 C11 C13 -78.2(2) . . . . ?
Pd1 P1 C11 C14 157.56(18) . . . . ?
Pd1 P1 C7 C9 49.81(19) . . . . ?
Pd1 P1 C7 C8 173.92(16) . . . . ?
Pd1 P1 C7 C10 -65.60(18) . . . . ?
Pd1 C1 C2 N2 0.7(3) . . . . ?
Pd1 C1 C2 C3 179.24(18) . . . . ?
Pd1 C1 C6 N1 4.7(3) . . . . ?
Pd1 C1 C6 C5 -175.72(19) . . . . ?
P2 N2 C2 C1 -7.7(3) . . . . ?
P2 N2 C2 C3 173.73(19) . . . . ?
P1 N1 C6 C1 -8.1(3) . . . . ?
P1 N1 C6 C5 172.3(2) . . . . ?
N2 P2 C15 C17 39.3(3) . . . . ?
N2 P2 C15 C16 164.0(2) . . . . ?
N2 P2 C15 C18 -77.7(2) . . . . ?
N2 P2 C19 C22 168.0(2) . . . . ?
N2 P2 C19 C21 52.0(2) . . . . ?
N2 P2 C19 C20 -67.5(2) . . . . ?
N2 C2 C3 C4 175.0(2) . . . . ?
N1 P1 C11 C12 -72.3(2) . . . . ?
N1 P1 C11 C13 170.6(2) . . . . ?
N1 P1 C11 C14 46.3(2) . . . . ?
N1 P1 C7 C9 161.95(18) . . . . ?
N1 P1 C7 C8 -73.9(2) . . . . ?
N1 P1 C7 C10 46.5(2) . . . . ?
N1 C6 C5 C4 176.1(2) . . . . ?
C1 C2 C3 C4 -3.5(4) . . . . ?
C1 C6 C5 C4 -3.5(4) . . . . ?
C2 C1 C6 N1 -177.3(2) . . . . ?
C2 C1 C6 C5 2.4(4) . . . . ?
C6 C1 C2 N2 -177.4(2) . . . . ?
C6 C1 C2 C3 1.2(4) . . . . ?
C6 C5 C4 C3 1.1(4) . . . . ?
C5 C4 C3 C2 2.3(4) . . . . ?
C11 P1 N1 C6 127.4(2) . . . . ?
C11 P1 C7 C9 -84.7(2) . . . . ?
C11 P1 C7 C8 39.4(2) . . . . ?
C11 P1 C7 C10 159.84(18) . . . . ?
C7 P1 N1 C6 -113.2(2) . . . . ?
C7 P1 C11 C12 173.10(18) . . . . ?
C7 P1 C11 C13 56.0(2) . . . . ?
C7 P1 C11 C14 -68.2(2) . . . . ?
C15 P2 N2 C2 130.9(2) . . . . ?
C15 P2 C19 C22 -78.7(2) . . . . ?
C15 P2 C19 C21 165.34(19) . . . . ?
C15 P2 C19 C20 45.8(3) . . . . ?
C19 P2 N2 C2 -109.4(2) . . . . ?
C19 P2 C15 C17 -74.6(3) . . . . ?
C19 P2 C15 C16 50.0(2) . . . . ?
C19 P2 C15 C18 168.37(19) . . . . ?

_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.750
