#------------------------------------------------------------------------------
#$Date: 2019-12-20 12:49:53 +0200 (Fri, 20 Dec 2019) $
#$Revision: 245433 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/66/1556697.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_1556697
loop_
_publ_author_name
'Messelberger, J.'
'Grunwald, A.'
'Stegner, P.'
'Senft, L.'
'Heinemann, F.W.'
'Munz, D.'
_publ_section_title
;
 Transmetalation from Magnesium-NHCs-Convenient Synthesis of Chelating
 pi-Acidic NHC Complexes
;
_journal_name_full               Inorganics
_journal_page_first              65
_journal_paper_doi               10.3390/inorganics7050065
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C43 H45 Br N5 Pd, Br'
_chemical_formula_sum            'C43 H45 Br2 N5 Pd'
_chemical_formula_weight         898.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 106.623(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.957(5)
_cell_length_b                   8.1726(17)
_cell_length_c                   22.929(5)
_cell_measurement_reflns_used    6940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.32
_cell_volume                     3763.0(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS high brilliance micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46711
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.162
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1133 before and 0.0711 after correction.
The Ratio of minimum to maximum transmission is 0.6130.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.567
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0694
_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)+(0.0491P)²+34.1566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1683
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5351
_reflns_number_total             7389
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Inorganics-2019-7-65.cif
_cod_data_source_block           dm1603
_cod_original_cell_volume        3763.1(14)
_cod_database_code               1556697
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.676
_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 Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C38(H38), C41(H41)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C34(H34), C35(H35),
  C36(H36)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
;
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'
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 0.45514(3) 0.39846(7) 0.68806(2) 0.01613(16) Uani 1 1 d . . . . .
Br1 Br 0.39799(4) 0.27131(11) 0.75269(4) 0.0301(2) Uani 1 1 d . . . . .
Br2 Br 0.55055(5) 0.14359(12) 0.60800(4) 0.0405(3) Uani 1 1 d . . . . .
N1 N 0.5862(3) 0.3530(7) 0.7981(3) 0.0166(13) Uani 1 1 d . . . . .
N2 N 0.5906(3) 0.4952(7) 0.7196(3) 0.0170(13) Uani 1 1 d . . . . .
N3 N 0.5001(3) 0.5239(7) 0.6375(3) 0.0160(13) Uani 1 1 d . . . . .
N4 N 0.3986(3) 0.5184(7) 0.5681(3) 0.0163(13) Uani 1 1 d . . . . .
N5 N 0.3147(3) 0.3947(7) 0.5867(2) 0.0156(12) Uani 1 1 d . . . . .
C1 C 0.5490(4) 0.4074(9) 0.7451(3) 0.0187(15) Uani 1 1 d . . . . .
C2 C 0.6531(3) 0.4035(9) 0.8086(3) 0.0184(15) Uani 1 1 d . . . . .
C3 C 0.7081(4) 0.3792(10) 0.8584(3) 0.0252(18) Uani 1 1 d . . . . .
H3 H 0.7060 0.3145 0.8923 0.030 Uiso 1 1 calc R . . . .
C4 C 0.7661(4) 0.4551(10) 0.8557(4) 0.0251(18) Uani 1 1 d . . . . .
H4 H 0.8049 0.4428 0.8891 0.030 Uiso 1 1 calc R . . . .
C5 C 0.7701(4) 0.5484(10) 0.8064(3) 0.0237(17) Uani 1 1 d . . . . .
H5 H 0.8111 0.5987 0.8068 0.028 Uiso 1 1 calc R . . . .
C6 C 0.7152(4) 0.5687(9) 0.7569(3) 0.0214(16) Uani 1 1 d . . . . .
H6 H 0.7180 0.6314 0.7228 0.026 Uiso 1 1 calc R . . . .
C7 C 0.6555(3) 0.4954(9) 0.7578(3) 0.0179(15) Uani 1 1 d . . . . .
C8 C 0.5648(4) 0.5593(9) 0.6603(3) 0.0186(16) Uani 1 1 d . . . . .
C9 C 0.5969(4) 0.6518(10) 0.6272(3) 0.0226(17) Uani 1 1 d . . . . .
H9 H 0.6427 0.6784 0.6431 0.027 Uiso 1 1 calc R . . . .
C10 C 0.5605(4) 0.7051(10) 0.5702(3) 0.0236(17) Uani 1 1 d . . . . .
H10 H 0.5815 0.7710 0.5470 0.028 Uiso 1 1 calc R . . . .
C11 C 0.4940(4) 0.6642(9) 0.5464(3) 0.0213(16) Uani 1 1 d . . . . .
H11 H 0.4692 0.6988 0.5069 0.026 Uiso 1 1 calc R . . . .
C12 C 0.4654(3) 0.5728(8) 0.5816(3) 0.0173(15) Uani 1 1 d . . . . .
C13 C 0.3456(3) 0.5396(8) 0.5156(3) 0.0154(15) Uani 1 1 d . . . . .
C14 C 0.3376(4) 0.6194(9) 0.4601(3) 0.0217(16) Uani 1 1 d . . . . .
H14 H 0.3735 0.6746 0.4510 0.026 Uiso 1 1 calc R . . . .
C15 C 0.2754(4) 0.6138(10) 0.4195(3) 0.0281(18) Uani 1 1 d . . . . .
H15 H 0.2683 0.6646 0.3809 0.034 Uiso 1 1 calc R . . . .
C16 C 0.2218(4) 0.5359(10) 0.4328(3) 0.0264(18) Uani 1 1 d . . . . .
H16 H 0.1792 0.5381 0.4036 0.032 Uiso 1 1 calc R . . . .
C17 C 0.2293(4) 0.4566(10) 0.4869(3) 0.0237(17) Uani 1 1 d . . . . .
H17 H 0.1932 0.4016 0.4958 0.028 Uiso 1 1 calc R . . . .
C18 C 0.2917(4) 0.4610(9) 0.5276(3) 0.0176(15) Uani 1 1 d . . . . .
C19 C 0.3791(3) 0.4301(8) 0.6121(3) 0.0150(15) Uani 1 1 d . . . . .
C20 C 0.5664(3) 0.2495(9) 0.8409(3) 0.0198(16) Uani 1 1 d . . . . .
C21 C 0.5555(4) 0.0845(10) 0.8277(3) 0.0253(18) Uani 1 1 d . . . . .
C22 C 0.5414(4) -0.0134(10) 0.8721(4) 0.0271(18) Uani 1 1 d . . . . .
H22 H 0.5332 -0.1269 0.8645 0.032 Uiso 1 1 calc R . . . .
C23 C 0.5391(4) 0.0515(10) 0.9264(4) 0.0294(19) Uani 1 1 d . . . . .
H23 H 0.5308 -0.0183 0.9565 0.035 Uiso 1 1 calc R . . . .
C24 C 0.5485(4) 0.2147(10) 0.9380(3) 0.0269(18) Uani 1 1 d . . . . .
H24 H 0.5464 0.2567 0.9760 0.032 Uiso 1 1 calc R . . . .
C25 C 0.5610(4) 0.3207(10) 0.8951(3) 0.0226(17) Uani 1 1 d . . . . .
C26 C 0.5591(4) 0.0079(10) 0.7683(4) 0.031(2) Uani 1 1 d . . . . .
H26 H 0.5540 0.0969 0.7374 0.037 Uiso 1 1 calc R . . . .
C27 C 0.5039(5) -0.1174(13) 0.7440(5) 0.057(3) Uani 1 1 d . . . . .
H27A H 0.4640 -0.0845 0.7552 0.085 Uiso 1 1 calc GR . . . .
H27B H 0.5188 -0.2250 0.7615 0.085 Uiso 1 1 calc GR . . . .
H27C H 0.4934 -0.1232 0.6995 0.085 Uiso 1 1 calc GR . . . .
C28 C 0.6261(4) -0.0746(12) 0.7763(4) 0.039(2) Uani 1 1 d . . . . .
H28A H 0.6619 0.0058 0.7908 0.059 Uiso 1 1 calc GR . . . .
H28B H 0.6281 -0.1194 0.7372 0.059 Uiso 1 1 calc GR . . . .
H28C H 0.6317 -0.1633 0.8061 0.059 Uiso 1 1 calc GR . . . .
C29 C 0.5639(4) 0.5031(9) 0.9061(4) 0.0254(18) Uani 1 1 d . . . . .
H29 H 0.5779 0.5563 0.8724 0.030 Uiso 1 1 calc R . . . .
C30 C 0.6147(5) 0.5489(13) 0.9663(4) 0.051(3) Uani 1 1 d . . . . .
H30A H 0.6589 0.5100 0.9662 0.076 Uiso 1 1 calc GR . . . .
H30B H 0.6021 0.4980 1.0001 0.076 Uiso 1 1 calc GR . . . .
H30C H 0.6157 0.6681 0.9712 0.076 Uiso 1 1 calc GR . . . .
C31 C 0.4949(5) 0.5634(11) 0.9028(5) 0.042(2) Uani 1 1 d . . . . .
H31A H 0.4652 0.5442 0.8618 0.063 Uiso 1 1 calc GR . . . .
H31B H 0.4966 0.6808 0.9118 0.063 Uiso 1 1 calc GR . . . .
H31C H 0.4782 0.5043 0.9326 0.063 Uiso 1 1 calc GR . . . .
C32 C 0.2722(3) 0.2898(9) 0.6102(3) 0.0174(15) Uani 1 1 d . . . . .
C33 C 0.2827(4) 0.1224(9) 0.6088(3) 0.0231(17) Uani 1 1 d . . . . .
C34 C 0.2379(4) 0.0229(11) 0.6271(3) 0.0277(18) Uani 1 1 d . . . . .
H34 H 0.2427 -0.0927 0.6268 0.033 Uiso 1 1 calc R . . . .
C35 C 0.1865(4) 0.0912(11) 0.6454(4) 0.0309(19) Uani 1 1 d . . . . .
H35 H 0.1559 0.0213 0.6568 0.037 Uiso 1 1 calc R . . . .
C36 C 0.1786(4) 0.2559(10) 0.6475(4) 0.0274(18) Uani 1 1 d . . . . .
H36 H 0.1434 0.2993 0.6614 0.033 Uiso 1 1 calc R . . . .
C37 C 0.2220(3) 0.3624(9) 0.6293(3) 0.0217(17) Uani 1 1 d . . . . .
C38 C 0.3401(4) 0.0482(10) 0.5893(4) 0.0304(19) Uani 1 1 d . . . . .
H38 H 0.3793 0.1218 0.6057 0.037 Uiso 1 1 calc R . . . .
C39 C 0.3280(5) 0.0430(11) 0.5213(4) 0.039(2) Uani 1 1 d . . . . .
H39A H 0.3693 0.0134 0.5120 0.058 Uiso 1 1 calc GR . . . .
H39B H 0.3130 0.1508 0.5040 0.058 Uiso 1 1 calc GR . . . .
H39C H 0.2936 -0.0387 0.5036 0.058 Uiso 1 1 calc GR . . . .
C40 C 0.3604(4) -0.1188(11) 0.6169(4) 0.035(2) Uani 1 1 d . . . . .
H40A H 0.4019 -0.1527 0.6086 0.053 Uiso 1 1 calc GR . . . .
H40B H 0.3252 -0.1982 0.5989 0.053 Uiso 1 1 calc GR . . . .
H40C H 0.3673 -0.1138 0.6609 0.053 Uiso 1 1 calc GR . . . .
C41 C 0.2148(4) 0.5451(10) 0.6339(3) 0.0233(17) Uani 1 1 d . . . . .
H41 H 0.2421 0.5980 0.6098 0.028 Uiso 1 1 calc R . . . .
C42 C 0.1426(4) 0.6026(11) 0.6075(4) 0.0298(19) Uani 1 1 d . . . . .
H42A H 0.1241 0.5561 0.5668 0.045 Uiso 1 1 calc GR . . . .
H42B H 0.1415 0.7223 0.6049 0.045 Uiso 1 1 calc GR . . . .
H42C H 0.1161 0.5662 0.6340 0.045 Uiso 1 1 calc GR . . . .
C43 C 0.2435(4) 0.5957(11) 0.6998(4) 0.0320(19) Uani 1 1 d . . . . .
H43A H 0.2905 0.5637 0.7140 0.048 Uiso 1 1 calc GR . . . .
H43B H 0.2188 0.5414 0.7247 0.048 Uiso 1 1 calc GR . . . .
H43C H 0.2398 0.7146 0.7033 0.048 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N3 Pd1 Br1 174.50(17) . .
N3 Pd1 C1 79.7(3) . .
N3 Pd1 C19 79.5(3) . .
C1 Pd1 Br1 100.5(2) . .
C19 Pd1 Br1 100.3(2) . .
C19 Pd1 C1 159.2(3) . .
C1 N1 C2 110.7(6) . .
C1 N1 C20 127.9(6) . .
C2 N1 C20 121.3(6) . .
C1 N2 C7 110.9(6) . .
C1 N2 C8 119.1(6) . .
C7 N2 C8 129.8(6) . .
C8 N3 Pd1 118.9(5) . .
C8 N3 C12 121.4(6) . .
C12 N3 Pd1 119.7(5) . .
C13 N4 C12 130.1(6) . .
C19 N4 C12 118.6(6) . .
C19 N4 C13 111.3(6) . .
C18 N5 C32 120.5(6) . .
C19 N5 C18 111.1(6) . .
C19 N5 C32 128.1(6) . .
N1 C1 Pd1 142.2(6) . .
N1 C1 N2 106.6(6) . .
N2 C1 Pd1 111.1(5) . .
C3 C2 N1 130.4(7) . .
C3 C2 C7 123.0(7) . .
C7 C2 N1 106.6(6) . .
C2 C3 H3 122.2 . .
C4 C3 C2 115.7(8) . .
C4 C3 H3 122.2 . .
C3 C4 H4 118.6 . .
C3 C4 C5 122.9(7) . .
C5 C4 H4 118.6 . .
C4 C5 H5 119.7 . .
C6 C5 C4 120.5(7) . .
C6 C5 H5 119.7 . .
C5 C6 H6 120.7 . .
C5 C6 C7 118.6(7) . .
C7 C6 H6 120.7 . .
N2 C7 C2 105.1(6) . .
N2 C7 C6 135.4(7) . .
C6 C7 C2 119.3(6) . .
N3 C8 N2 111.2(6) . .
N3 C8 C9 120.3(6) . .
C9 C8 N2 128.5(7) . .
C8 C9 H9 120.9 . .
C8 C9 C10 118.1(7) . .
C10 C9 H9 120.9 . .
C9 C10 H10 119.4 . .
C9 C10 C11 121.2(7) . .
C11 C10 H10 119.4 . .
C10 C11 H11 121.2 . .
C12 C11 C10 117.6(7) . .
C12 C11 H11 121.2 . .
N3 C12 N4 110.4(6) . .
N3 C12 C11 121.4(6) . .
C11 C12 N4 128.2(6) . .
N4 C13 C14 134.5(7) . .
C18 C13 N4 105.2(6) . .
C18 C13 C14 120.2(6) . .
C13 C14 H14 121.8 . .
C15 C14 C13 116.5(7) . .
C15 C14 H14 121.8 . .
C14 C15 H15 118.8 . .
C14 C15 C16 122.3(7) . .
C16 C15 H15 118.8 . .
C15 C16 H16 119.2 . .
C17 C16 C15 121.5(7) . .
C17 C16 H16 119.2 . .
C16 C17 H17 121.8 . .
C16 C17 C18 116.4(7) . .
C18 C17 H17 121.8 . .
C13 C18 N5 107.1(6) . .
C17 C18 N5 129.9(7) . .
C17 C18 C13 123.1(7) . .
N4 C19 Pd1 111.8(5) . .
N5 C19 Pd1 143.0(5) . .
N5 C19 N4 105.2(5) . .
C21 C20 N1 118.8(7) . .
C21 C20 C25 123.1(7) . .
C25 C20 N1 118.1(7) . .
C20 C21 C22 117.1(7) . .
C20 C21 C26 123.3(7) . .
C22 C21 C26 119.6(7) . .
C21 C22 H22 119.6 . .
C23 C22 C21 120.9(8) . .
C23 C22 H22 119.6 . .
C22 C23 H23 119.4 . .
C24 C23 C22 121.1(8) . .
C24 C23 H23 119.4 . .
C23 C24 H24 119.4 . .
C23 C24 C25 121.1(8) . .
C25 C24 H24 119.4 . .
C20 C25 C29 123.1(7) . .
C24 C25 C20 116.5(7) . .
C24 C25 C29 120.3(7) . .
C21 C26 H26 108.3 . .
C21 C26 C27 112.2(8) . .
C21 C26 C28 110.8(7) . .
C27 C26 H26 108.3 . .
C28 C26 H26 108.3 . .
C28 C26 C27 108.9(7) . .
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27B 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C26 C28 H28A 109.5 . .
C26 C28 H28B 109.5 . .
C26 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C25 C29 H29 107.9 . .
C25 C29 C30 112.1(7) . .
C30 C29 H29 107.9 . .
C31 C29 C25 108.7(7) . .
C31 C29 H29 107.9 . .
C31 C29 C30 112.0(8) . .
C29 C30 H30A 109.5 . .
C29 C30 H30B 109.5 . .
C29 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C29 C31 H31A 109.5 . .
C29 C31 H31B 109.5 . .
C29 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C33 C32 N5 117.3(7) . .
C37 C32 N5 117.9(6) . .
C37 C32 C33 124.6(7) . .
C32 C33 C34 116.4(7) . .
C32 C33 C38 122.8(7) . .
C34 C33 C38 120.8(7) . .
C33 C34 H34 119.8 . .
C35 C34 C33 120.4(8) . .
C35 C34 H34 119.8 . .
C34 C35 H35 119.1 . .
C36 C35 C34 121.8(8) . .
C36 C35 H35 119.1 . .
C35 C36 H36 119.8 . .
C35 C36 C37 120.4(8) . .
C37 C36 H36 119.8 . .
C32 C37 C36 116.4(7) . .
C32 C37 C41 123.1(7) . .
C36 C37 C41 120.4(7) . .
C33 C38 H38 106.4 . .
C39 C38 C33 113.7(7) . .
C39 C38 H38 106.4 . .
C39 C38 C40 110.5(7) . .
C40 C38 C33 112.8(7) . .
C40 C38 H38 106.4 . .
C38 C39 H39A 109.5 . .
C38 C39 H39B 109.5 . .
C38 C39 H39C 109.5 . .
H39A C39 H39B 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
C38 C40 H40A 109.5 . .
C38 C40 H40B 109.5 . .
C38 C40 H40C 109.5 . .
H40A C40 H40B 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
C37 C41 H41 107.8 . .
C37 C41 C42 112.6(6) . .
C37 C41 C43 108.6(6) . .
C42 C41 H41 107.8 . .
C43 C41 H41 107.8 . .
C43 C41 C42 112.0(7) . .
C41 C42 H42A 109.5 . .
C41 C42 H42B 109.5 . .
C41 C42 H42C 109.5 . .
H42A C42 H42B 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C41 C43 H43A 109.5 . .
C41 C43 H43B 109.5 . .
C41 C43 H43C 109.5 . .
H43A C43 H43B 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Br1 2.3929(10) .
Pd1 N3 1.977(6) .
Pd1 C1 2.027(7) .
Pd1 C19 2.012(7) .
N1 C1 1.321(9) .
N1 C2 1.415(9) .
N1 C20 1.444(9) .
N2 C1 1.380(9) .
N2 C7 1.392(9) .
N2 C8 1.413(9) .
N3 C8 1.338(9) .
N3 C12 1.340(9) .
N4 C12 1.417(9) .
N4 C13 1.395(9) .
N4 C19 1.394(9) .
N5 C18 1.410(9) .
N5 C19 1.340(9) .
N5 C32 1.446(9) .
C2 C3 1.385(10) .
C2 C7 1.400(10) .
C3 H3 0.9500 .
C3 C4 1.382(11) .
C4 H4 0.9500 .
C4 C5 1.387(11) .
C5 H5 0.9500 .
C5 C6 1.376(10) .
C6 H6 0.9500 .
C6 C7 1.393(10) .
C8 C9 1.374(10) .
C9 H9 0.9500 .
C9 C10 1.381(10) .
C10 H10 0.9500 .
C10 C11 1.385(10) .
C11 H11 0.9500 .
C11 C12 1.359(10) .
C13 C14 1.398(10) .
C13 C18 1.392(10) .
C14 H14 0.9500 .
C14 C15 1.370(11) .
C15 H15 0.9500 .
C15 C16 1.398(11) .
C16 H16 0.9500 .
C16 C17 1.368(11) .
C17 H17 0.9500 .
C17 C18 1.374(10) .
C20 C21 1.387(11) .
C20 C25 1.405(11) .
C21 C22 1.391(11) .
C21 C26 1.520(11) .
C22 H22 0.9500 .
C22 C23 1.367(12) .
C23 H23 0.9500 .
C23 C24 1.363(12) .
C24 H24 0.9500 .
C24 C25 1.391(11) .
C25 C29 1.510(11) .
C26 H26 1.0000 .
C26 C27 1.526(12) .
C26 C28 1.522(12) .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29 1.0000 .
C29 C30 1.529(12) .
C29 C31 1.509(12) .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 C33 1.387(11) .
C32 C37 1.385(11) .
C33 C34 1.394(11) .
C33 C38 1.525(11) .
C34 H34 0.9500 .
C34 C35 1.380(12) .
C35 H35 0.9500 .
C35 C36 1.359(12) .
C36 H36 0.9500 .
C36 C37 1.406(11) .
C37 C41 1.507(11) .
C38 H38 1.0000 .
C38 C39 1.507(12) .
C38 C40 1.513(12) .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C40 H40A 0.9800 .
C40 H40B 0.9800 .
C40 H40C 0.9800 .
C41 H41 1.0000 .
C41 C42 1.534(10) .
C41 C43 1.516(11) .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
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
Pd1 N3 C8 N2 0.6(8) . . . .
Pd1 N3 C8 C9 -177.4(6) . . . .
Pd1 N3 C12 N4 -1.2(8) . . . .
Pd1 N3 C12 C11 177.6(6) . . . .
N1 C2 C3 C4 -175.7(7) . . . .
N1 C2 C7 N2 -0.1(7) . . . .
N1 C2 C7 C6 176.7(6) . . . .
N1 C20 C21 C22 175.3(6) . . . .
N1 C20 C21 C26 -4.0(11) . . . .
N1 C20 C25 C24 -173.6(6) . . . .
N1 C20 C25 C29 10.3(10) . . . .
N2 C8 C9 C10 -178.1(7) . . . .
N3 C8 C9 C10 -0.5(11) . . . .
N4 C13 C14 C15 -179.0(8) . . . .
N4 C13 C18 N5 -0.4(7) . . . .
N4 C13 C18 C17 179.0(7) . . . .
N5 C32 C33 C34 -175.0(6) . . . .
N5 C32 C33 C38 5.6(10) . . . .
N5 C32 C37 C36 175.3(6) . . . .
N5 C32 C37 C41 -7.5(10) . . . .
C1 N1 C2 C3 177.7(8) . . . .
C1 N1 C2 C7 0.1(8) . . . .
C1 N1 C20 C21 74.3(10) . . . .
C1 N1 C20 C25 -107.6(8) . . . .
C1 N2 C7 C2 0.0(8) . . . .
C1 N2 C7 C6 -176.0(8) . . . .
C1 N2 C8 N3 0.9(9) . . . .
C1 N2 C8 C9 178.7(7) . . . .
C2 N1 C1 Pd1 176.2(7) . . . .
C2 N1 C1 N2 -0.2(8) . . . .
C2 N1 C20 C21 -102.6(8) . . . .
C2 N1 C20 C25 75.5(9) . . . .
C2 C3 C4 C5 -0.7(11) . . . .
C3 C2 C7 N2 -177.8(7) . . . .
C3 C2 C7 C6 -1.0(11) . . . .
C3 C4 C5 C6 -0.4(12) . . . .
C4 C5 C6 C7 0.8(11) . . . .
C5 C6 C7 N2 175.5(8) . . . .
C5 C6 C7 C2 -0.1(11) . . . .
C7 N2 C1 Pd1 -177.5(5) . . . .
C7 N2 C1 N1 0.1(8) . . . .
C7 N2 C8 N3 175.6(7) . . . .
C7 N2 C8 C9 -6.6(13) . . . .
C7 C2 C3 C4 1.4(11) . . . .
C8 N2 C1 Pd1 -1.8(8) . . . .
C8 N2 C1 N1 175.8(6) . . . .
C8 N2 C7 C2 -175.1(7) . . . .
C8 N2 C7 C6 8.9(13) . . . .
C8 N3 C12 N4 179.3(6) . . . .
C8 N3 C12 C11 -1.8(11) . . . .
C8 C9 C10 C11 -1.2(12) . . . .
C9 C10 C11 C12 1.4(12) . . . .
C10 C11 C12 N3 0.1(11) . . . .
C10 C11 C12 N4 178.7(7) . . . .
C12 N3 C8 N2 180.0(6) . . . .
C12 N3 C8 C9 2.0(11) . . . .
C12 N4 C13 C14 -1.2(13) . . . .
C12 N4 C13 C18 -179.8(7) . . . .
C12 N4 C19 Pd1 -0.4(8) . . . .
C12 N4 C19 N5 -179.5(6) . . . .
C13 N4 C12 N3 -179.4(6) . . . .
C13 N4 C12 C11 1.8(12) . . . .
C13 N4 C19 Pd1 180.0(4) . . . .
C13 N4 C19 N5 0.9(8) . . . .
C13 C14 C15 C16 1.4(12) . . . .
C14 C13 C18 N5 -179.3(6) . . . .
C14 C13 C18 C17 0.1(11) . . . .
C14 C15 C16 C17 -1.9(13) . . . .
C15 C16 C17 C18 1.3(12) . . . .
C16 C17 C18 N5 178.7(7) . . . .
C16 C17 C18 C13 -0.5(11) . . . .
C18 N5 C19 Pd1 -179.7(7) . . . .
C18 N5 C19 N4 -1.2(8) . . . .
C18 N5 C32 C33 100.3(8) . . . .
C18 N5 C32 C37 -76.4(8) . . . .
C18 C13 C14 C15 -0.5(10) . . . .
C19 N4 C12 N3 1.1(9) . . . .
C19 N4 C12 C11 -177.7(7) . . . .
C19 N4 C13 C14 178.3(8) . . . .
C19 N4 C13 C18 -0.3(8) . . . .
C19 N5 C18 C13 1.0(8) . . . .
C19 N5 C18 C17 -178.3(8) . . . .
C19 N5 C32 C33 -72.8(9) . . . .
C19 N5 C32 C37 110.4(8) . . . .
C20 N1 C1 Pd1 -1.0(13) . . . .
C20 N1 C1 N2 -177.4(6) . . . .
C20 N1 C2 C3 -4.9(12) . . . .
C20 N1 C2 C7 177.6(6) . . . .
C20 C21 C22 C23 -0.6(11) . . . .
C20 C21 C26 C27 -139.2(8) . . . .
C20 C21 C26 C28 98.9(9) . . . .
C20 C25 C29 C30 -128.5(8) . . . .
C20 C25 C29 C31 107.1(9) . . . .
C21 C20 C25 C24 4.4(11) . . . .
C21 C20 C25 C29 -171.7(7) . . . .
C21 C22 C23 C24 2.1(12) . . . .
C22 C21 C26 C27 41.5(10) . . . .
C22 C21 C26 C28 -80.4(9) . . . .
C22 C23 C24 C25 -0.3(12) . . . .
C23 C24 C25 C20 -2.8(11) . . . .
C23 C24 C25 C29 173.4(7) . . . .
C24 C25 C29 C30 55.6(10) . . . .
C24 C25 C29 C31 -68.9(9) . . . .
C25 C20 C21 C22 -2.7(11) . . . .
C25 C20 C21 C26 178.0(7) . . . .
C26 C21 C22 C23 178.8(7) . . . .
C32 N5 C18 C13 -173.2(6) . . . .
C32 N5 C18 C17 7.5(11) . . . .
C32 N5 C19 Pd1 -6.0(13) . . . .
C32 N5 C19 N4 172.5(6) . . . .
C32 C33 C34 C35 -0.2(11) . . . .
C32 C33 C38 C39 -78.9(10) . . . .
C32 C33 C38 C40 154.2(7) . . . .
C32 C37 C41 C42 135.3(7) . . . .
C32 C37 C41 C43 -100.0(8) . . . .
C33 C32 C37 C36 -1.2(11) . . . .
C33 C32 C37 C41 176.0(7) . . . .
C33 C34 C35 C36 -1.3(12) . . . .
C34 C33 C38 C39 101.7(9) . . . .
C34 C33 C38 C40 -25.2(10) . . . .
C34 C35 C36 C37 1.7(13) . . . .
C35 C36 C37 C32 -0.5(11) . . . .
C35 C36 C37 C41 -177.8(7) . . . .
C36 C37 C41 C42 -47.6(10) . . . .
C36 C37 C41 C43 77.0(8) . . . .
C37 C32 C33 C34 1.5(11) . . . .
C37 C32 C33 C38 -177.9(7) . . . .
C38 C33 C34 C35 179.2(7) . . . .
