#------------------------------------------------------------------------------
#$Date: 2022-03-01 04:09:22 +0200 (Tue, 01 Mar 2022) $
#$Revision: 273189 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/45/7244528.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7244528
loop_
_publ_author_name
'Morla, Jhansi Rani'
'Nareddula, Dastagiri Reddy'
_publ_section_title
;
 Synthesis of dihydroisoquinolinone-4-methylboronic esters via domino
 Heck/borylation using a structurally characterized palladacycle as a
 catalyst
;
_journal_issue                   11
_journal_name_full               'RSC Advances'
_journal_page_first              6762
_journal_page_last               6771
_journal_paper_doi               10.1039/D2RA00389A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C37 H29 Cl N5 O P Pd, 2(C3 H6 O)'
_chemical_formula_sum            'C43 H41 Cl N5 O3 P Pd'
_chemical_formula_weight         848.63
_chemical_name_systematic        Palladacycle
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-05-31T12:03:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2021-06-02 deposited with the CCDC.	2022-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.477(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5617(4)
_cell_length_b                   39.7290(15)
_cell_length_c                   10.2744(4)
_cell_measurement_reflns_used    9303
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.0274
_cell_measurement_theta_min      3.9173
_cell_volume                     3899.4(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0060303
_diffrn_orient_matrix_UB_12      -0.0147065
_diffrn_orient_matrix_UB_13      0.0384031
_diffrn_orient_matrix_UB_21      -0.0189738
_diffrn_orient_matrix_UB_22      -0.0093839
_diffrn_orient_matrix_UB_23      -0.0567314
_diffrn_orient_matrix_UB_31      0.0715106
_diffrn_orient_matrix_UB_32      -0.0037366
_diffrn_orient_matrix_UB_33      -0.0087908
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29580
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.104
_diffrn_reflns_theta_min         3.929
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.92838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
        (compiled Sep 14 2012,17:21:16)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN and acetone'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.243
_refine_diff_density_min         -3.942
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.1159
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+110.0319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2373
_reflns_Friedel_coverage         0
_reflns_number_gt                7615
_reflns_number_total             9220
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra00389a2.cif
_cod_data_source_block           Palladacycle
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7244528
_shelx_shelxl_version_number     2018/3
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
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 0.72398(7) 0.36337(2) 0.76281(6) 0.01372(15) Uani 1 1 d . . . . .
P1 P 0.7235(2) 0.41272(5) 0.6395(2) 0.0127(4) Uani 1 1 d . . . . .
N2 N 0.5927(7) 0.32975(16) 0.9741(7) 0.0144(14) Uani 1 1 d . . . . .
C1 C 0.6926(8) 0.32271(18) 0.8886(7) 0.0099(14) Uiso 1 1 d . . . . .
N3 N 0.4655(8) 0.37112(17) 1.0804(7) 0.0222(16) Uani 1 1 d . . . . .
N4 N 0.5626(7) 0.41705(17) 0.8922(7) 0.0180(14) Uani 1 1 d . . . . .
N1 N 0.7284(7) 0.29127(17) 0.9080(7) 0.0166(14) Uani 1 1 d . . . . .
C32 C 0.8370(8) 0.4448(2) 0.7113(8) 0.0170(16) Uani 1 1 d . . . . .
C31 C 0.5133(10) 0.4636(2) 0.6297(9) 0.0243(19) Uani 1 1 d . . . . .
H31 H 0.582261 0.4792 0.653413 0.029 Uiso 1 1 calc R U . . .
C3 C 0.5468(8) 0.3632(2) 0.9859(8) 0.0193(16) Uani 1 1 d . . . . .
C26 C 0.5488(8) 0.4303(2) 0.6138(8) 0.0179(17) Uani 1 1 d . . . . .
C5 C 0.4719(8) 0.4271(2) 0.9867(8) 0.0160(16) Uani 1 1 d . . . . .
C23 C 0.9006(11) 0.4133(2) 0.2266(9) 0.030(2) Uani 1 1 d . . . . .
H23 H 0.937832 0.4134 0.144428 0.036 Uiso 1 1 calc R U . . .
C37 C 0.9041(10) 0.4391(3) 0.8359(9) 0.027(2) Uani 1 1 d . . . . .
H37 H 0.881674 0.420124 0.883554 0.032 Uiso 1 1 calc R U . . .
C35 C 1.0340(11) 0.4901(3) 0.8174(11) 0.035(2) Uani 1 1 d . . . . .
H35 H 1.100525 0.50506 0.852047 0.042 Uiso 1 1 calc R U . . .
C34 C 0.9687(10) 0.4969(2) 0.6969(10) 0.027(2) Uani 1 1 d . . . . .
H34 H 0.98978 0.516383 0.651772 0.033 Uiso 1 1 calc R U . . .
C29 C 0.2721(10) 0.4513(3) 0.5731(11) 0.037(3) Uani 1 1 d . . . . .
H29 H 0.180194 0.458542 0.55863 0.044 Uiso 1 1 calc R U . . .
C24 C 0.7621(12) 0.4218(3) 0.2415(11) 0.037(2) Uani 1 1 d . . . . .
H24 H 0.706357 0.428423 0.169709 0.044 Uiso 1 1 calc R U . . .
C2 C 0.5981(8) 0.3857(2) 0.8889(8) 0.0159(16) Uani 1 1 d . . . . .
C11 C 0.6499(9) 0.2769(2) 1.0060(8) 0.0193(17) Uani 1 1 d . . . . .
H11 H 0.654826 0.25486 1.035921 0.023 Uiso 1 1 calc R U . . .
C28 C 0.3059(10) 0.4179(3) 0.5573(10) 0.036(2) Uani 1 1 d . . . . .
H28 H 0.23663 0.402446 0.532662 0.043 Uiso 1 1 calc R U . . .
C22 C 0.9838(10) 0.4047(2) 0.3363(10) 0.028(2) Uani 1 1 d . . . . .
H22 H 1.077754 0.399499 0.327517 0.033 Uiso 1 1 calc R U . . .
C33 C 0.8712(9) 0.4741(2) 0.6448(9) 0.0212(18) Uani 1 1 d . . . . .
H33 H 0.827903 0.478422 0.563796 0.025 Uiso 1 1 calc R U . . .
C7 C 0.3409(10) 0.4711(2) 1.0862(10) 0.031(2) Uani 1 1 d . . . . .
H7 H 0.309114 0.493272 1.086273 0.037 Uiso 1 1 calc R U . . .
C27 C 0.4430(9) 0.4073(2) 0.5781(9) 0.0236(19) Uani 1 1 d . . . . .
H27 H 0.465061 0.38469 0.568188 0.028 Uiso 1 1 calc R U . . .
C25 C 0.7053(10) 0.4202(3) 0.3654(9) 0.030(2) Uani 1 1 d . . . . .
H25 H 0.610966 0.425061 0.374243 0.036 Uiso 1 1 calc R U . . .
C6 C 0.4254(10) 0.4606(2) 0.9900(9) 0.0242(19) Uani 1 1 d . . . . .
H6 H 0.452106 0.475697 0.92651 0.029 Uiso 1 1 calc R U . . .
C20 C 0.7874(8) 0.4117(2) 0.4737(7) 0.0146(15) Uani 1 1 d . . . . .
C9 C 0.3431(11) 0.4167(3) 1.1812(11) 0.037(3) Uani 1 1 d . . . . .
H9 H 0.314743 0.402149 1.245878 0.044 Uiso 1 1 calc R U . . .
C0AA C 0.5661(10) 0.3014(2) 1.0481(8) 0.0218(18) Uani 1 1 d . . . . .
H0AA H 0.502741 0.299714 1.113964 0.026 Uiso 1 1 calc R U . . .
C4 C 0.4275(9) 0.4046(2) 1.0834(9) 0.0208(18) Uani 1 1 d . . . . .
C8 C 0.3022(12) 0.4495(3) 1.1829(11) 0.038(3) Uani 1 1 d . . . . .
H8 H 0.247907 0.457247 1.249571 0.045 Uiso 1 1 calc R U . . .
C30 C 0.3753(11) 0.4740(3) 0.6105(10) 0.035(2) Uani 1 1 d . . . . .
H30 H 0.352317 0.496518 0.623033 0.042 Uiso 1 1 calc R U . . .
C36 C 1.0019(11) 0.4616(3) 0.8864(11) 0.037(3) Uani 1 1 d . . . . .
H36 H 1.046402 0.457496 0.967136 0.045 Uiso 1 1 calc R U . . .
C21 C 0.9284(9) 0.4038(2) 0.4571(9) 0.0208(18) Uani 1 1 d . . . . .
H21 H 0.985303 0.3979 0.529151 0.025 Uiso 1 1 calc R U . . .
Cl1 Cl 0.8667(3) 0.33342(6) 0.6183(2) 0.0277(5) Uani 1 1 d . . . . .
O1 O 0.6520(6) 0.24341(16) 0.7294(7) 0.0265(15) Uani 1 1 d . . . . .
N13 N 0.8782(7) 0.22868(19) 0.6943(8) 0.0226(16) Uani 1 1 d . . . . .
H13 H 0.961505 0.23078 0.728254 0.027 Uiso 1 1 calc R U . . .
C14 C 0.8636(10) 0.2063(2) 0.5876(9) 0.0244(19) Uani 1 1 d . . . . .
C12 C 0.8386(8) 0.2731(2) 0.8446(9) 0.0177(16) Uani 1 1 d . . . . .
H12A H 0.898308 0.261984 0.910114 0.021 Uiso 1 1 calc R U . . .
H12B H 0.895658 0.288929 0.798343 0.021 Uiso 1 1 calc R U . . .
O2 O 0.9601(11) 0.2707(3) 0.1635(10) 0.066(3) Uani 1 1 d . . . . .
C15 C 0.9852(11) 0.1958(2) 0.5319(11) 0.033(2) Uani 1 1 d . . . . .
H15 H 1.071972 0.202127 0.568394 0.039 Uiso 1 1 calc R U . . .
C19 C 0.7346(12) 0.1951(3) 0.5382(12) 0.039(3) Uani 1 1 d . . . . .
H19 H 0.652885 0.201009 0.578438 0.046 Uiso 1 1 calc R U . . .
C16 C 0.9766(15) 0.1756(3) 0.4200(12) 0.050(3) Uani 1 1 d . . . . .
H16 H 1.058051 0.168509 0.382097 0.06 Uiso 1 1 calc R U . . .
C43 C 0.1760(15) 0.3209(3) 0.9667(15) 0.056(4) Uani 1 1 d . . . . .
H43A H 0.269934 0.315954 0.943619 0.084 Uiso 1 1 calc R U . . .
H43B H 0.111763 0.306688 0.918024 0.084 Uiso 1 1 calc R U . . .
H43C H 0.166973 0.317065 1.058214 0.084 Uiso 1 1 calc R U . . .
C18 C 0.7294(16) 0.1748(3) 0.4262(13) 0.055(4) Uani 1 1 d . . . . .
H18 H 0.643682 0.16695 0.392355 0.066 Uiso 1 1 calc R U . . .
O3 O 0.079(2) 0.3735(5) 1.0176(17) 0.149(7) Uani 1 1 d . . . . .
C13 C 0.7787(9) 0.2472(2) 0.7499(9) 0.0189(17) Uani 1 1 d . . . . .
C17 C 0.8503(17) 0.1664(3) 0.3668(12) 0.055(4) Uani 1 1 d . . . . .
H17 H 0.845565 0.154354 0.289198 0.066 Uiso 1 1 calc R U . . .
C38 C 0.8624(16) 0.3230(3) 0.2422(12) 0.053(4) Uani 1 1 d . . . . .
H38A H 0.923437 0.334091 0.184035 0.079 Uiso 1 1 calc R U . . .
H38B H 0.879537 0.331432 0.328929 0.079 Uiso 1 1 calc R U . . .
H38C H 0.766806 0.327224 0.214715 0.079 Uiso 1 1 calc R U . . .
C39 C 0.8905(13) 0.2848(3) 0.2402(12) 0.045(3) Uani 1 1 d . . . . .
C40 C 0.817(2) 0.2665(4) 0.3399(15) 0.083(6) Uani 1 1 d . . . . .
H40A H 0.844161 0.243245 0.339327 0.125 Uiso 1 1 calc R U . . .
H40B H 0.717477 0.268122 0.321811 0.125 Uiso 1 1 calc R U . . .
H40C H 0.839618 0.276035 0.423924 0.125 Uiso 1 1 calc R U . . .
C41 C 0.1821(17) 0.3770(4) 0.8266(15) 0.081(6) Uani 1 1 d . . . . .
H41A H 0.269077 0.368914 0.795293 0.122 Uiso 1 1 calc R U . . .
H41B H 0.192524 0.400083 0.852949 0.122 Uiso 1 1 calc R U . . .
H41C H 0.110499 0.375337 0.758497 0.122 Uiso 1 1 calc R U . . .
C42 C 0.144(2) 0.3571(6) 0.936(2) 0.092(6) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pd1 C1 80.7(3) . . ?
C2 Pd1 P1 89.5(2) . . ?
C1 Pd1 P1 169.7(2) . . ?
C2 Pd1 Cl1 176.2(2) . . ?
C1 Pd1 Cl1 95.8(2) . . ?
P1 Pd1 Cl1 93.97(8) . . ?
C32 P1 C26 108.7(4) . . ?
C32 P1 C20 100.1(4) . . ?
C26 P1 C20 102.4(4) . . ?
C32 P1 Pd1 112.5(3) . . ?
C26 P1 Pd1 112.4(3) . . ?
C20 P1 Pd1 119.6(3) . . ?
C1 N2 C0AA 109.8(6) . . ?
C1 N2 C3 118.9(6) . . ?
C0AA N2 C3 130.8(7) . . ?
N1 C1 N2 106.6(7) . . ?
N1 C1 Pd1 141.8(6) . . ?
N2 C1 Pd1 111.3(5) . . ?
C3 N3 C4 114.4(7) . . ?
C2 N4 C5 117.8(7) . . ?
C1 N1 C11 110.6(7) . . ?
C1 N1 C12 126.6(7) . . ?
C11 N1 C12 122.7(7) . . ?
C33 C32 C37 117.7(8) . . ?
C33 C32 P1 122.4(7) . . ?
C37 C32 P1 119.7(7) . . ?
C26 C31 C30 120.5(10) . . ?
C26 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
N3 C3 N2 119.3(7) . . ?
N3 C3 C2 126.6(8) . . ?
N2 C3 C2 114.2(7) . . ?
C31 C26 C27 118.6(8) . . ?
C31 C26 P1 125.5(7) . . ?
C27 C26 P1 115.9(7) . . ?
N4 C5 C6 119.7(8) . . ?
N4 C5 C4 121.8(7) . . ?
C6 C5 C4 118.5(7) . . ?
C24 C23 C22 119.1(9) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C36 C37 C32 120.6(9) . . ?
C36 C37 H37 119.7 . . ?
C32 C37 H37 119.7 . . ?
C36 C35 C34 121.1(9) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C34 C33 119.0(9) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
C28 C29 C30 119.6(9) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C23 C24 C25 120.0(10) . . ?
C23 C24 H24 120 . . ?
C25 C24 H24 120 . . ?
N4 C2 C3 118.9(7) . . ?
N4 C2 Pd1 127.4(6) . . ?
C3 C2 Pd1 113.7(6) . . ?
C0AA C11 N1 106.4(7) . . ?
C0AA C11 H11 126.8 . . ?
N1 C11 H11 126.8 . . ?
C29 C28 C27 120.0(10) . . ?
C29 C28 H28 120 . . ?
C27 C28 H28 120 . . ?
C21 C22 C23 120.6(9) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C34 C33 C32 121.5(9) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C6 C7 C8 121.0(9) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C28 C27 C26 120.8(9) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C20 C25 C24 120.9(9) . . ?
C20 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C7 C6 C5 120.3(9) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C25 C20 C21 118.3(8) . . ?
C25 C20 P1 123.0(7) . . ?
C21 C20 P1 118.6(6) . . ?
C8 C9 C4 120.9(9) . . ?
C8 C9 H9 119.6 . . ?
C4 C9 H9 119.6 . . ?
C11 C0AA N2 106.5(7) . . ?
C11 C0AA H0AA 126.7 . . ?
N2 C0AA H0AA 126.7 . . ?
N3 C4 C9 120.5(8) . . ?
N3 C4 C5 120.4(7) . . ?
C9 C4 C5 119.1(8) . . ?
C9 C8 C7 120.2(9) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C29 C30 C31 120.5(10) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C37 C36 C35 120.1(10) . . ?
C37 C36 H36 120 . . ?
C35 C36 H36 120 . . ?
C22 C21 C20 121.1(8) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C13 N13 C14 128.6(8) . . ?
C13 N13 H13 115.7 . . ?
C14 N13 H13 115.7 . . ?
C15 C14 C19 120.3(9) . . ?
C15 C14 N13 117.0(8) . . ?
C19 C14 N13 122.7(8) . . ?
N1 C12 C13 111.4(7) . . ?
N1 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
N1 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108 . . ?
C14 C15 C16 119.4(11) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C14 C19 C18 118.9(11) . . ?
C14 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C17 C16 C15 120.4(11) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C17 C18 C19 120.2(12) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
O1 C13 N13 124.6(8) . . ?
O1 C13 C12 122.4(8) . . ?
N13 C13 C12 112.9(7) . . ?
C16 C17 C18 120.6(11) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O2 C39 C40 121.9(14) . . ?
O2 C39 C38 125.0(13) . . ?
C40 C39 C38 113.0(12) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O3 C42 C41 113(2) . . ?
O3 C42 C43 117.7(19) . . ?
C41 C42 C43 129.4(19) . . ?
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 C2 2.013(8) . ?
Pd1 C1 2.099(7) . ?
Pd1 P1 2.334(2) . ?
Pd1 Cl1 2.378(2) . ?
P1 C32 1.809(9) . ?
P1 C26 1.819(8) . ?
P1 C20 1.835(8) . ?
N2 C1 1.354(9) . ?
N2 C0AA 1.388(10) . ?
N2 C3 1.408(10) . ?
C1 N1 1.308(9) . ?
N3 C3 1.307(10) . ?
N3 C4 1.379(10) . ?
N4 C2 1.291(10) . ?
N4 C5 1.388(10) . ?
N1 C11 1.403(10) . ?
N1 C12 1.454(10) . ?
C32 C33 1.396(12) . ?
C32 C37 1.424(12) . ?
C31 C26 1.378(12) . ?
C31 C30 1.389(13) . ?
C31 H31 0.93 . ?
C3 C2 1.441(11) . ?
C26 C27 1.399(12) . ?
C5 C6 1.406(11) . ?
C5 C4 1.414(12) . ?
C23 C24 1.381(15) . ?
C23 C22 1.395(15) . ?
C23 H23 0.93 . ?
C37 C36 1.378(13) . ?
C37 H37 0.93 . ?
C35 C36 1.378(15) . ?
C35 C34 1.388(15) . ?
C35 H35 0.93 . ?
C34 C33 1.390(12) . ?
C34 H34 0.93 . ?
C29 C28 1.378(16) . ?
C29 C30 1.379(16) . ?
C29 H29 0.93 . ?
C24 C25 1.406(14) . ?
C24 H24 0.93 . ?
C11 C0AA 1.343(12) . ?
C11 H11 0.93 . ?
C28 C27 1.385(12) . ?
C28 H28 0.93 . ?
C22 C21 1.370(12) . ?
C22 H22 0.93 . ?
C33 H33 0.93 . ?
C7 C6 1.369(13) . ?
C7 C8 1.378(15) . ?
C7 H7 0.93 . ?
C27 H27 0.93 . ?
C25 C20 1.376(12) . ?
C25 H25 0.93 . ?
C6 H6 0.93 . ?
C20 C21 1.402(11) . ?
C9 C8 1.359(14) . ?
C9 C4 1.401(12) . ?
C9 H9 0.93 . ?
C0AA H0AA 0.93 . ?
C8 H8 0.93 . ?
C30 H30 0.93 . ?
C36 H36 0.93 . ?
C21 H21 0.93 . ?
O1 C13 1.230(10) . ?
N13 C13 1.348(10) . ?
N13 C14 1.415(11) . ?
N13 H13 0.86 . ?
C14 C15 1.381(13) . ?
C14 C19 1.386(14) . ?
C12 C13 1.512(12) . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
O2 C39 1.193(14) . ?
C15 C16 1.401(15) . ?
C15 H15 0.93 . ?
C19 C18 1.404(16) . ?
C19 H19 0.93 . ?
C16 C17 1.354(19) . ?
C16 H16 0.93 . ?
C43 C42 1.50(2) . ?
C43 H43A 0.96 . ?
C43 H43B 0.96 . ?
C43 H43C 0.96 . ?
C18 C17 1.372(19) . ?
C18 H18 0.93 . ?
O3 C42 1.25(2) . ?
C17 H17 0.93 . ?
C38 C39 1.540(17) . ?
C38 H38A 0.96 . ?
C38 H38B 0.96 . ?
C38 H38C 0.96 . ?
C39 C40 1.464(19) . ?
C40 H40A 0.96 . ?
C40 H40B 0.96 . ?
C40 H40C 0.96 . ?
C41 C42 1.44(2) . ?
C41 H41A 0.96 . ?
C41 H41B 0.96 . ?
C41 H41C 0.96 . ?
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
C0AA N2 C1 N1 -0.3(9) . . . . ?
C3 N2 C1 N1 172.3(7) . . . . ?
C0AA N2 C1 Pd1 174.9(6) . . . . ?
C3 N2 C1 Pd1 -12.5(9) . . . . ?
N2 C1 N1 C11 1.0(9) . . . . ?
Pd1 C1 N1 C11 -171.7(7) . . . . ?
N2 C1 N1 C12 -175.8(7) . . . . ?
Pd1 C1 N1 C12 11.5(14) . . . . ?
C26 P1 C32 C33 -65.7(8) . . . . ?
C20 P1 C32 C33 41.2(8) . . . . ?
Pd1 P1 C32 C33 169.2(6) . . . . ?
C26 P1 C32 C37 119.7(7) . . . . ?
C20 P1 C32 C37 -133.5(7) . . . . ?
Pd1 P1 C32 C37 -5.4(8) . . . . ?
C4 N3 C3 N2 179.6(8) . . . . ?
C4 N3 C3 C2 0.2(13) . . . . ?
C1 N2 C3 N3 -170.4(8) . . . . ?
C0AA N2 C3 N3 0.3(14) . . . . ?
C1 N2 C3 C2 9.1(11) . . . . ?
C0AA N2 C3 C2 179.9(8) . . . . ?
C30 C31 C26 C27 0.0(13) . . . . ?
C30 C31 C26 P1 -178.3(7) . . . . ?
C32 P1 C26 C31 8.1(9) . . . . ?
C20 P1 C26 C31 -97.2(8) . . . . ?
Pd1 P1 C26 C31 133.3(7) . . . . ?
C32 P1 C26 C27 -170.2(6) . . . . ?
C20 P1 C26 C27 84.5(7) . . . . ?
Pd1 P1 C26 C27 -45.1(7) . . . . ?
C2 N4 C5 C6 -177.1(8) . . . . ?
C2 N4 C5 C4 4.9(12) . . . . ?
C33 C32 C37 C36 -1.6(14) . . . . ?
P1 C32 C37 C36 173.2(8) . . . . ?
C36 C35 C34 C33 -1.2(15) . . . . ?
C22 C23 C24 C25 -2.6(15) . . . . ?
C5 N4 C2 C3 -2.5(12) . . . . ?
C5 N4 C2 Pd1 178.8(6) . . . . ?
N3 C3 C2 N4 0.0(14) . . . . ?
N2 C3 C2 N4 -179.5(8) . . . . ?
N3 C3 C2 Pd1 178.9(7) . . . . ?
N2 C3 C2 Pd1 -0.6(9) . . . . ?
C1 N1 C11 C0AA -1.4(10) . . . . ?
C12 N1 C11 C0AA 175.6(8) . . . . ?
C30 C29 C28 C27 -0.4(16) . . . . ?
C24 C23 C22 C21 1.5(15) . . . . ?
C35 C34 C33 C32 0.6(13) . . . . ?
C37 C32 C33 C34 0.8(13) . . . . ?
P1 C32 C33 C34 -173.9(7) . . . . ?
C29 C28 C27 C26 -0.7(15) . . . . ?
C31 C26 C27 C28 0.9(13) . . . . ?
P1 C26 C27 C28 179.4(7) . . . . ?
C23 C24 C25 C20 2.6(16) . . . . ?
C8 C7 C6 C5 1.4(16) . . . . ?
N4 C5 C6 C7 -177.1(9) . . . . ?
C4 C5 C6 C7 1.0(14) . . . . ?
C24 C25 C20 C21 -1.5(14) . . . . ?
C24 C25 C20 P1 174.8(8) . . . . ?
C32 P1 C20 C25 -116.9(8) . . . . ?
C26 P1 C20 C25 -5.0(9) . . . . ?
Pd1 P1 C20 C25 119.9(7) . . . . ?
C32 P1 C20 C21 59.4(7) . . . . ?
C26 P1 C20 C21 171.3(7) . . . . ?
Pd1 P1 C20 C21 -63.8(7) . . . . ?
N1 C11 C0AA N2 1.2(10) . . . . ?
C1 N2 C0AA C11 -0.6(10) . . . . ?
C3 N2 C0AA C11 -172.0(8) . . . . ?
C3 N3 C4 C9 -178.6(9) . . . . ?
C3 N3 C4 C5 2.2(13) . . . . ?
C8 C9 C4 N3 -178.3(11) . . . . ?
C8 C9 C4 C5 1.0(17) . . . . ?
N4 C5 C4 N3 -4.9(13) . . . . ?
C6 C5 C4 N3 177.1(8) . . . . ?
N4 C5 C4 C9 175.9(9) . . . . ?
C6 C5 C4 C9 -2.2(14) . . . . ?
C4 C9 C8 C7 1.4(19) . . . . ?
C6 C7 C8 C9 -2.6(18) . . . . ?
C28 C29 C30 C31 1.4(16) . . . . ?
C26 C31 C30 C29 -1.1(15) . . . . ?
C32 C37 C36 C35 1.1(16) . . . . ?
C34 C35 C36 C37 0.3(17) . . . . ?
C23 C22 C21 C20 -0.4(14) . . . . ?
C25 C20 C21 C22 0.4(13) . . . . ?
P1 C20 C21 C22 -176.1(7) . . . . ?
C13 N13 C14 C15 166.7(9) . . . . ?
C13 N13 C14 C19 -12.7(16) . . . . ?
C1 N1 C12 C13 -109.2(9) . . . . ?
C11 N1 C12 C13 74.4(10) . . . . ?
C19 C14 C15 C16 4.1(16) . . . . ?
N13 C14 C15 C16 -175.3(9) . . . . ?
C15 C14 C19 C18 -3.8(17) . . . . ?
N13 C14 C19 C18 175.5(11) . . . . ?
C14 C15 C16 C17 0.0(18) . . . . ?
C14 C19 C18 C17 -1(2) . . . . ?
C14 N13 C13 O1 12.6(16) . . . . ?
C14 N13 C13 C12 -168.8(8) . . . . ?
N1 C12 C13 O1 1.8(12) . . . . ?
N1 C12 C13 N13 -176.8(7) . . . . ?
C15 C16 C17 C18 -4(2) . . . . ?
C19 C18 C17 C16 5(2) . . . . ?
