#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/14/4111456.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_4111456
loop_
_publ_author_name
'Laurent F. Groux'
'Thomas Weiss'
'Dastigiri N. Reddy'
'Preston A. Chase'
'Warren E. Piers'
'Tom Ziegler'
'Masood Parvez'
'Jordi Benet-Buchholz'
_publ_contact_author
;
    Masood Parvez
    Department of Chemistry
    University of Calgary
    2500 University Drive N.W.
    Calgary, Alberta, Canada T2N 1N4
;
_publ_contact_author_email       parvez@ucalgary.ca
_publ_contact_author_fax         (403)289-9488
_publ_contact_author_phone       (403)220-5348
_publ_section_title
;
 Insertion of Acrylonitrile into Palladium Methyl Bonds in Neutral and
 Anionic Pd(II) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1854
_journal_page_last               1869
_journal_paper_doi               10.1021/ja044119+
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C30.5 H45.5 N3 O Pd'
_chemical_formula_weight         576.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.220(4)
_cell_angle_beta                 110.871(3)
_cell_angle_gamma                98.433(3)
_cell_formula_units_Z            4
_cell_length_a                   13.9617(12)
_cell_length_b                   14.0737(11)
_cell_length_c                   17.2592(14)
_cell_measurement_temperature    153(2)
_cell_volume                     3112.9(4)
_computing_cell_refinement       'Bruker SAINT program Vers. 5.0'
_computing_data_collection       'Bruker SMART CCD area detector system'
_computing_data_reduction        'Bruker SAINT program Vers. 5.0'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            'Smart 1000 CCD area detector'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'four-circle diffractometer Bruker P4'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans,
 in omega at 0.3 deg scan width, three runs with 98, 67 and 67 frames, phi=0 deg
 in phi at 0.3 deg scan width, two runs with 1207 frames, omega=-32 deg
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_sigmaI/netI    0.2159
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46750
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.47
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           250
_diffrn_source_power             47
_diffrn_source_size              '10 mm x 0.5 mm fine focus'
_diffrn_source_type              'MACScience Co. M18X-HF'
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.670673
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Siemens SADABS program multi-scan
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       needle
_exptl_crystal_F_000             1214
_exptl_crystal_preparation
;
 Slow evaporation of dichloromethane under inert conditions
;
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.544
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.773
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         18397
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.772
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0281P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                8089
_reflns_number_total             18397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0441192Bsi20040927_052928.cif
_cod_data_source_block           1a-NCCH3
_cod_original_formula_sum        'C30.50 H45.50 N3 O Pd'
_cod_database_code               4111456
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.52335(2) -0.08414(2) 0.67036(2) 0.02477(9) Uani 1 1 d . . .
N1 N 0.5014(3) -0.0771(2) 0.7775(2) 0.0216(8) Uani 1 1 d . . .
O1 O 0.3666(2) -0.0936(2) 0.60615(17) 0.0286(7) Uani 1 1 d . . .
C1 C 0.2959(3) -0.1069(3) 0.6371(2) 0.0242(9) Uani 1 1 d . . .
N2 N 0.4141(3) -0.0935(2) 0.7879(2) 0.0223(8) Uani 1 1 d . . .
C2 C 0.3176(3) -0.1114(3) 0.7241(2) 0.0206(9) Uani 1 1 d . . .
N3 N 0.5332(3) -0.1035(3) 0.5569(2) 0.0313(9) Uani 1 1 d . . .
C3 C 0.2365(3) -0.1333(3) 0.7550(2) 0.0218(9) Uani 1 1 d . . .
H3A H 0.2537 -0.1357 0.8132 0.026 Uiso 1 1 calc R . .
C4 C 0.1342(3) -0.1510(3) 0.7028(2) 0.0240(9) Uani 1 1 d . . .
C5 C 0.1134(3) -0.1401(3) 0.6176(3) 0.0273(10) Uani 1 1 d . . .
H5A H 0.0424 -0.1485 0.5814 0.033 Uiso 1 1 calc R . .
C6 C 0.1875(3) -0.1183(3) 0.5826(2) 0.0225(9) Uani 1 1 d . . .
C7 C 0.0440(3) -0.1791(3) 0.7316(3) 0.0342(11) Uani 1 1 d . . .
C8 C 0.0796(4) -0.1944(4) 0.8229(3) 0.0438(13) Uani 1 1 d . . .
H8A H 0.1199 -0.1338 0.8572 0.066 Uiso 1 1 calc R . .
H8B H 0.1233 -0.2443 0.8331 0.066 Uiso 1 1 calc R . .
H8C H 0.0187 -0.2151 0.8375 0.066 Uiso 1 1 calc R . .
C9 C -0.0235(5) -0.1032(5) 0.7159(4) 0.088(2) Uani 1 1 d . . .
H9A H 0.0151 -0.0435 0.7525 0.132 Uiso 1 1 calc R . .
H9B H -0.0863 -0.1259 0.7275 0.132 Uiso 1 1 calc R . .
H9C H -0.0434 -0.0906 0.6575 0.132 Uiso 1 1 calc R . .
C10 C -0.0212(4) -0.2751(5) 0.6821(4) 0.082(2) Uani 1 1 d . . .
H10A H -0.0786 -0.2947 0.7012 0.123 Uiso 1 1 calc R . .
H10B H 0.0228 -0.3249 0.6909 0.123 Uiso 1 1 calc R . .
H10C H -0.0494 -0.2674 0.6226 0.123 Uiso 1 1 calc R . .
C11 C 0.1594(3) -0.1073(3) 0.4905(2) 0.0271(9) Uani 1 1 d . . .
C12 C 0.0412(3) -0.1186(4) 0.4444(3) 0.0392(12) Uani 1 1 d . . .
H12A H 0.0076 -0.1835 0.4482 0.059 Uiso 1 1 calc R . .
H12B H 0.0260 -0.1095 0.3856 0.059 Uiso 1 1 calc R . .
H12C H 0.0145 -0.0701 0.4701 0.059 Uiso 1 1 calc R . .
C13 C 0.2078(4) -0.0057(3) 0.4794(3) 0.0396(12) Uani 1 1 d . . .
H13A H 0.2836 0.0046 0.5085 0.059 Uiso 1 1 calc R . .
H13B H 0.1793 0.0432 0.5029 0.059 Uiso 1 1 calc R . .
H13C H 0.1913 -0.0004 0.4199 0.059 Uiso 1 1 calc R . .
C14 C 0.1974(4) -0.1840(4) 0.4486(3) 0.0418(13) Uani 1 1 d . . .
H14A H 0.2735 -0.1754 0.4741 0.063 Uiso 1 1 calc R . .
H14B H 0.1766 -0.1774 0.3889 0.063 Uiso 1 1 calc R . .
H14C H 0.1667 -0.2484 0.4560 0.063 Uiso 1 1 calc R . .
C15 C 0.5860(3) -0.0594(3) 0.8586(3) 0.0239(10) Uani 1 1 d . . .
C16 C 0.6313(3) -0.1365(3) 0.8929(2) 0.0227(9) Uani 1 1 d . . .
C17 C 0.7125(3) -0.1180(3) 0.9694(3) 0.0313(10) Uani 1 1 d . . .
H17A H 0.7451 -0.1694 0.9939 0.038 Uiso 1 1 calc R . .
C18 C 0.7467(3) -0.0250(3) 1.0105(3) 0.0390(12) Uani 1 1 d . . .
H18A H 0.8016 -0.0129 1.0638 0.047 Uiso 1 1 calc R . .
C19 C 0.7018(4) 0.0492(4) 0.9749(3) 0.0428(13) Uani 1 1 d . . .
H19A H 0.7278 0.1128 1.0034 0.051 Uiso 1 1 calc R . .
C20 C 0.6203(3) 0.0357(3) 0.8991(3) 0.0375(12) Uani 1 1 d . . .
C21 C 0.5908(3) -0.2394(3) 0.8515(3) 0.0318(10) Uani 1 1 d . . .
H21A H 0.5402 -0.2374 0.7938 0.038 Uiso 1 1 calc R . .
C22 C 0.6773(4) -0.2902(4) 0.8438(3) 0.0506(14) Uani 1 1 d . . .
H22A H 0.6482 -0.3578 0.8204 0.076 Uiso 1 1 calc R . .
H22B H 0.7316 -0.2877 0.8991 0.076 Uiso 1 1 calc R . .
H22C H 0.7075 -0.2575 0.8070 0.076 Uiso 1 1 calc R . .
C23 C 0.5329(4) -0.2973(3) 0.8979(3) 0.0472(13) Uani 1 1 d . . .
H23A H 0.5162 -0.3657 0.8752 0.071 Uiso 1 1 calc R . .
H23B H 0.4683 -0.2732 0.8911 0.071 Uiso 1 1 calc R . .
H23C H 0.5767 -0.2904 0.9573 0.071 Uiso 1 1 calc R . .
C24 C 0.5704(4) 0.1201(4) 0.8619(3) 0.0537(15) Uani 1 1 d . . .
H24A H 0.5068 0.0942 0.8113 0.064 Uiso 1 1 calc R . .
C25 C 0.6461(5) 0.1883(4) 0.8359(4) 0.0731(19) Uani 1 1 d . . .
H25A H 0.6605 0.1544 0.7912 0.110 Uiso 1 1 calc R . .
H25B H 0.7112 0.2097 0.8840 0.110 Uiso 1 1 calc R . .
H25C H 0.6151 0.2447 0.8158 0.110 Uiso 1 1 calc R . .
C26 C 0.5378(5) 0.1757(4) 0.9256(4) 0.076(2) Uani 1 1 d . . .
H26A H 0.5014 0.2268 0.8994 0.114 Uiso 1 1 calc R . .
H26B H 0.6000 0.2046 0.9741 0.114 Uiso 1 1 calc R . .
H26C H 0.4914 0.1309 0.9436 0.114 Uiso 1 1 calc R . .
C27 C 0.6803(3) -0.0659(4) 0.7225(3) 0.0452(13) Uani 1 1 d . . .
H27A H 0.7029 -0.0492 0.7830 0.068 Uiso 1 1 calc R . .
H27B H 0.7111 -0.0138 0.6987 0.068 Uiso 1 1 calc R . .
H27C H 0.7031 -0.1261 0.7111 0.068 Uiso 1 1 calc R . .
C28 C 0.5251(3) -0.1203(3) 0.4894(3) 0.0328(11) Uani 1 1 d . . .
C29 C 0.5103(4) -0.1439(3) 0.4029(3) 0.0404(12) Uani 1 1 d . . .
H29A H 0.4373 -0.1453 0.3678 0.061 Uiso 1 1 calc R . .
H29B H 0.5286 -0.2075 0.3954 0.061 Uiso 1 1 calc R . .
H29C H 0.5550 -0.0949 0.3868 0.061 Uiso 1 1 calc R . .
Pd1B Pd 0.60554(2) -0.37268(2) 0.398336(19) 0.02095(9) Uani 1 1 d . . .
N1B N 0.6386(2) -0.3942(2) 0.29697(19) 0.0188(7) Uani 1 1 d . . .
O1B O 0.4493(2) -0.4197(2) 0.33028(16) 0.0254(7) Uani 1 1 d . . .
C1B C 0.4075(3) -0.4344(3) 0.2507(2) 0.0185(8) Uani 1 1 d . . .
N2B N 0.5739(2) -0.4174(2) 0.2219(2) 0.0196(8) Uani 1 1 d . . .
C2B C 0.4672(3) -0.4330(3) 0.1980(2) 0.0183(8) Uani 1 1 d . . .
N3B N 0.5657(3) -0.3563(3) 0.4981(2) 0.0291(9) Uani 1 1 d . . .
C3B C 0.4159(3) -0.4512(3) 0.1095(2) 0.0192(8) Uani 1 1 d . . .
H3BA H 0.4569 -0.4514 0.0758 0.023 Uiso 1 1 calc R . .
C4B C 0.3105(3) -0.4681(3) 0.0715(2) 0.0194(8) Uani 1 1 d . . .
C5B C 0.2533(3) -0.4695(3) 0.1245(2) 0.0234(9) Uani 1 1 d . . .
H5BA H 0.1795 -0.4812 0.0989 0.028 Uiso 1 1 calc R . .
C6B C 0.2962(3) -0.4554(3) 0.2107(2) 0.0199(8) Uani 1 1 d . . .
C7B C 0.2524(3) -0.4861(3) -0.0230(2) 0.0294(10) Uani 1 1 d . . .
C8B C 0.1747(4) -0.5818(4) -0.0468(3) 0.0452(14) Uani 1 1 d . . .
H8BA H 0.1231 -0.5784 -0.0208 0.068 Uiso 1 1 calc R . .
H8BB H 0.2120 -0.6349 -0.0271 0.068 Uiso 1 1 calc R . .
H8BC H 0.1393 -0.5934 -0.1076 0.068 Uiso 1 1 calc R . .
C9B C 0.1902(4) -0.4065(4) -0.0519(3) 0.0580(16) Uani 1 1 d . . .
H9BA H 0.2376 -0.3441 -0.0384 0.087 Uiso 1 1 calc R . .
H9BB H 0.1407 -0.4050 -0.0237 0.087 Uiso 1 1 calc R . .
H9BC H 0.1521 -0.4190 -0.1124 0.087 Uiso 1 1 calc R . .
C10B C 0.3264(4) -0.4933(4) -0.0686(3) 0.0527(15) Uani 1 1 d . . .
H10D H 0.3786 -0.4339 -0.0535 0.079 Uiso 1 1 calc R . .
H10E H 0.2871 -0.5020 -0.1290 0.079 Uiso 1 1 calc R . .
H10F H 0.3612 -0.5488 -0.0528 0.079 Uiso 1 1 calc R . .
C11B C 0.2282(3) -0.4611(3) 0.2638(3) 0.0291(10) Uani 1 1 d . . .
C12B C 0.2558(4) -0.5373(4) 0.3247(3) 0.0404(12) Uani 1 1 d . . .
H12D H 0.2488 -0.5999 0.2934 0.061 Uiso 1 1 calc R . .
H12E H 0.2085 -0.5432 0.3554 0.061 Uiso 1 1 calc R . .
H12F H 0.3277 -0.5175 0.3643 0.061 Uiso 1 1 calc R . .
C13B C 0.2450(4) -0.3628(3) 0.3132(3) 0.0411(12) Uani 1 1 d . . .
H13D H 0.2262 -0.3143 0.2745 0.062 Uiso 1 1 calc R . .
H13E H 0.3184 -0.3444 0.3500 0.062 Uiso 1 1 calc R . .
H13F H 0.2012 -0.3666 0.3468 0.062 Uiso 1 1 calc R . .
C14B C 0.1123(3) -0.4890(4) 0.2096(3) 0.0443(13) Uani 1 1 d . . .
H14D H 0.0912 -0.4388 0.1732 0.066 Uiso 1 1 calc R . .
H14E H 0.0715 -0.4954 0.2455 0.066 Uiso 1 1 calc R . .
H14F H 0.1000 -0.5508 0.1754 0.066 Uiso 1 1 calc R . .
C15B C 0.7447(3) -0.3817(3) 0.2987(2) 0.0218(9) Uani 1 1 d . . .
C16B C 0.8036(3) -0.4533(3) 0.3302(3) 0.0321(10) Uani 1 1 d . . .
C17B C 0.9041(4) -0.4405(4) 0.3309(3) 0.0470(14) Uani 1 1 d . . .
H17B H 0.9461 -0.4877 0.3514 0.056 Uiso 1 1 calc R . .
C18B C 0.9445(3) -0.3607(4) 0.3026(3) 0.0507(15) Uani 1 1 d . . .
H18B H 1.0138 -0.3532 0.3039 0.061 Uiso 1 1 calc R . .
C19B C 0.8852(3) -0.2920(4) 0.2724(3) 0.0373(12) Uani 1 1 d . . .
H19B H 0.8821 -0.2868 0.2146 0.045 Uiso 1 1 calc R . .
H19C H 0.9243 -0.2295 0.3056 0.045 Uiso 1 1 calc R . .
C20B C 0.7843(3) -0.3001(3) 0.2701(2) 0.0253(9) Uani 1 1 d . . .
C21B C 0.7578(4) -0.5417(3) 0.3599(3) 0.0447(13) Uani 1 1 d . . .
H21B H 0.6994 -0.5252 0.3757 0.054 Uiso 1 1 calc R . .
C22B C 0.7137(5) -0.6232(4) 0.2905(4) 0.0740(19) Uani 1 1 d . . .
H22D H 0.6892 -0.6816 0.3114 0.111 Uiso 1 1 calc R . .
H22E H 0.7678 -0.6355 0.2693 0.111 Uiso 1 1 calc R . .
H22F H 0.6552 -0.6059 0.2453 0.111 Uiso 1 1 calc R . .
C23B C 0.8379(5) -0.5727(5) 0.4372(4) 0.095(3) Uani 1 1 d . . .
H23D H 0.8680 -0.5178 0.4811 0.142 Uiso 1 1 calc R . .
H23E H 0.8934 -0.5941 0.4221 0.142 Uiso 1 1 calc R . .
H23F H 0.8035 -0.6260 0.4575 0.142 Uiso 1 1 calc R . .
C24B C 0.7227(3) -0.2212(3) 0.2405(3) 0.0310(10) Uani 1 1 d . . .
H24B H 0.6473 -0.2519 0.2173 0.037 Uiso 1 1 calc R . .
C25B C 0.7378(5) -0.1478(4) 0.3123(4) 0.076(2) Uani 1 1 d . . .
H25D H 0.7190 -0.1802 0.3550 0.114 Uiso 1 1 calc R . .
H25E H 0.6933 -0.0996 0.2924 0.114 Uiso 1 1 calc R . .
H25F H 0.8109 -0.1156 0.3363 0.114 Uiso 1 1 calc R . .
C26B C 0.7454(6) -0.1721(5) 0.1719(4) 0.091(2) Uani 1 1 d . . .
H26D H 0.6952 -0.1292 0.1497 0.136 Uiso 1 1 calc R . .
H26E H 0.7398 -0.2210 0.1270 0.136 Uiso 1 1 calc R . .
H26F H 0.8161 -0.1340 0.1943 0.136 Uiso 1 1 calc R . .
C27B C 0.7542(3) -0.3204(4) 0.4744(3) 0.0381(12) Uani 1 1 d . . .
H27D H 0.7901 -0.3743 0.4940 0.057 Uiso 1 1 calc R . .
H27E H 0.7548 -0.2793 0.5224 0.057 Uiso 1 1 calc R . .
H27F H 0.7900 -0.2822 0.4437 0.057 Uiso 1 1 calc R . .
C28B C 0.5343(4) -0.3536(3) 0.5507(3) 0.0331(11) Uani 1 1 d . . .
C29B C 0.4924(4) -0.3483(4) 0.6167(3) 0.0527(14) Uani 1 1 d . . .
H29D H 0.5264 -0.2883 0.6542 0.079 Uiso 1 1 calc R . .
H29E H 0.5053 -0.4039 0.6483 0.079 Uiso 1 1 calc R . .
H29F H 0.4172 -0.3492 0.5919 0.079 Uiso 1 1 calc R . .
C1L C -0.036(5) 0.121(5) -0.112(4) 0.16(3) Uani 0.33 1 d PU A 1
H1LD H -0.0671 0.1792 -0.1247 0.240 Uiso 0.33 1 d PR A 1
H1LE H -0.0900 0.0634 -0.1352 0.240 Uiso 0.33 1 d PR A 1
H1LF H 0.0171 0.1202 -0.1371 0.240 Uiso 0.33 1 d PR A 1
C2L C -0.012(3) 0.105(3) -0.031(2) 0.075(11) Uani 0.33 1 d PU A 1
H2LC H -0.0555 0.1323 -0.0043 0.090 Uiso 0.33 1 d PR A 1
H2LD H 0.0595 0.1431 -0.0089 0.090 Uiso 0.33 1 d PR A 1
C3L C -0.012(2) 0.030(4) -0.029(4) 0.074(11) Uani 0.33 1 d PU . 1
C1L' C -0.046(3) 0.202(2) -0.115(3) 0.102(12) Uani 0.33 1 d PU B 2
H1LA H -0.0684 0.1861 -0.1760 0.152 Uiso 0.33 1 d PR B 2
H1LB H 0.0193 0.2492 -0.0951 0.152 Uiso 0.33 1 d PR B 2
H1LC H -0.0995 0.2292 -0.1022 0.152 Uiso 0.33 1 d PR B 2
C2L' C -0.037(4) 0.025(5) -0.062(3) 0.14(2) Uani 0.33 1 d PU . 2
H2LA H 0.0216 0.0514 -0.0779 0.171 Uiso 0.33 1 d PR . 2
H2LB H -0.1082 0.0292 -0.1000 0.171 Uiso 0.33 1 d PR . 2
C3L' C 0.019(3) 0.032(4) 0.025(3) 0.107(13) Uani 0.33 1 d PU . 2
H3LA H -0.0371 0.0560 0.0385 0.129 Uiso 0.33 1 d PR . 2
H3LB H 0.0850 0.0768 0.0593 0.129 Uiso 0.33 1 d PR . 2
C2L" C -0.020(3) 0.171(3) -0.043(3) 0.126(13) Uani 0.33 1 d PU C 3
C3L" C -0.031(4) 0.094(5) -0.071(4) 0.101(15) Uani 0.33 1 d PU C 3
C1L" C -0.059(4) 0.153(3) -0.139(3) 0.102(12) Uani 0.33 1 d PU C 3
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'
O O 0.0106 0.0060 '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
N1 Pd1 N3 173.93(14) . .
N1 Pd1 C27 95.45(17) . .
N3 Pd1 C27 88.89(18) . .
N1 Pd1 O1 90.36(12) . .
N3 Pd1 O1 85.61(13) . .
C27 Pd1 O1 173.06(17) . .
N2 N1 C15 109.1(3) . .
N2 N1 Pd1 127.2(3) . .
C15 N1 Pd1 123.5(3) . .
C1 O1 Pd1 125.9(2) . .
O1 C1 C2 123.4(3) . .
O1 C1 C6 119.5(4) . .
C2 C1 C6 117.2(4) . .
N1 N2 C2 124.6(3) . .
N2 C2 C3 111.4(3) . .
N2 C2 C1 127.1(4) . .
C3 C2 C1 121.5(3) . .
C28 N3 Pd1 170.7(4) . .
C4 C3 C2 121.4(4) . .
C3 C4 C5 116.7(4) . .
C3 C4 C7 123.8(4) . .
C5 C4 C7 119.5(3) . .
C6 C5 C4 125.5(4) . .
C5 C6 C1 117.5(4) . .
C5 C6 C11 122.7(3) . .
C1 C6 C11 119.8(4) . .
C9 C7 C8 109.4(4) . .
C9 C7 C4 110.0(4) . .
C8 C7 C4 112.8(3) . .
C9 C7 C10 108.9(5) . .
C8 C7 C10 106.7(4) . .
C4 C7 C10 108.8(4) . .
C6 C11 C14 110.5(3) . .
C6 C11 C12 111.7(4) . .
C14 C11 C12 107.6(3) . .
C6 C11 C13 110.3(3) . .
C14 C11 C13 109.8(4) . .
C12 C11 C13 106.9(4) . .
C16 C15 C20 122.3(4) . .
C16 C15 N1 119.1(3) . .
C20 C15 N1 118.7(3) . .
C17 C16 C15 118.2(4) . .
C17 C16 C21 119.5(4) . .
C15 C16 C21 122.2(3) . .
C16 C17 C18 120.3(4) . .
C19 C18 C17 120.1(4) . .
C18 C19 C20 122.5(4) . .
C19 C20 C15 116.6(4) . .
C19 C20 C24 121.1(4) . .
C15 C20 C24 122.3(4) . .
C16 C21 C23 110.8(4) . .
C16 C21 C22 112.5(4) . .
C23 C21 C22 110.1(4) . .
C20 C24 C25 110.1(5) . .
C20 C24 C26 110.4(5) . .
C25 C24 C26 110.0(5) . .
N3 C28 C29 177.6(5) . .
N1B Pd1B N3B 177.08(14) . .
N1B Pd1B C27B 94.96(16) . .
N3B Pd1B C27B 87.66(17) . .
N1B Pd1B O1B 90.78(12) . .
N3B Pd1B O1B 86.64(13) . .
C27B Pd1B O1B 173.99(16) . .
N2B N1B C15B 109.9(3) . .
N2B N1B Pd1B 127.1(3) . .
C15B N1B Pd1B 123.0(2) . .
C1B O1B Pd1B 125.5(2) . .
O1B C1B C6B 119.8(3) . .
O1B C1B C2B 122.9(3) . .
C6B C1B C2B 117.3(3) . .
N1B N2B C2B 125.0(3) . .
N2B C2B C3B 111.9(3) . .
N2B C2B C1B 127.8(3) . .
C3B C2B C1B 120.3(3) . .
C28B N3B Pd1B 173.1(4) . .
C4B C3B C2B 122.3(4) . .
C3B C4B C5B 116.5(3) . .
C3B C4B C7B 124.1(4) . .
C5B C4B C7B 119.5(3) . .
C6B C5B C4B 125.2(4) . .
C5B C6B C1B 118.4(3) . .
C5B C6B C11B 121.9(3) . .
C1B C6B C11B 119.8(3) . .
C10B C7B C9B 110.7(4) . .
C10B C7B C4B 111.6(3) . .
C9B C7B C4B 109.8(4) . .
C10B C7B C8B 107.2(4) . .
C9B C7B C8B 107.2(4) . .
C4B C7B C8B 110.3(4) . .
C13B C11B C14B 107.9(4) . .
C13B C11B C6B 109.7(3) . .
C14B C11B C6B 111.6(3) . .
C13B C11B C12B 109.3(4) . .
C14B C11B C12B 107.7(4) . .
C6B C11B C12B 110.5(3) . .
C20B C15B C16B 122.6(4) . .
C20B C15B N1B 119.6(4) . .
C16B C15B N1B 117.8(4) . .
C17B C16B C15B 117.1(4) . .
C17B C16B C21B 121.7(4) . .
C15B C16B C21B 121.2(4) . .
C18B C17B C16B 121.3(5) . .
C19B C18B C17B 120.3(4) . .
C18B C19B C20B 121.5(5) . .
C19B C20B C15B 117.3(4) . .
C19B C20B C24B 120.4(4) . .
C15B C20B C24B 122.3(4) . .
C22B C21B C16B 109.9(4) . .
C22B C21B C23B 110.6(5) . .
C16B C21B C23B 112.2(4) . .
C25B C24B C20B 110.7(4) . .
C25B C24B C26B 110.3(5) . .
C20B C24B C26B 114.0(4) . .
N3B C28B C29B 178.4(5) . .
C2L C1L C3L 31(3) . .
C3L C2L C1L 107(5) . .
C2L C3L C3L 138(9) . 2
C2L C3L C1L 42(4) . .
C3L C3L C1L 175(3) 2 .
C3L' C2L' C3L' 53(4) 2 .
C2L' C3L' C3L' 80(7) 2 2
C2L' C3L' C2L' 127(4) 2 .
C3L' C3L' C2L' 47(5) 2 .
C3L" C2L" C1L" 64(4) . .
C2L" C3L" C1L" 72(5) . .
C3L" C1L" C2L" 44(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 1.978(3) .
Pd1 N3 2.018(4) .
Pd1 C27 2.021(4) .
Pd1 O1 2.050(3) .
N1 N2 1.285(4) .
N1 C15 1.455(5) .
O1 C1 1.276(5) .
C1 C2 1.429(5) .
C1 C6 1.449(5) .
N2 C2 1.381(5) .
C2 C3 1.416(5) .
N3 C28 1.137(5) .
C3 C4 1.366(5) .
C4 C5 1.416(6) .
C4 C7 1.520(6) .
C5 C6 1.379(6) .
C6 C11 1.518(5) .
C7 C9 1.500(7) .
C7 C8 1.512(6) .
C7 C10 1.530(7) .
C11 C14 1.523(6) .
C11 C12 1.535(5) .
C11 C13 1.541(6) .
C15 C16 1.391(5) .
C15 C20 1.406(6) .
C16 C17 1.379(5) .
C16 C21 1.512(6) .
C17 C18 1.385(6) .
C18 C19 1.360(6) .
C19 C20 1.374(6) .
C20 C24 1.523(6) .
C21 C23 1.516(6) .
C21 C22 1.531(6) .
C24 C25 1.526(8) .
C24 C26 1.546(8) .
C28 C29 1.444(6) .
Pd1B N1B 1.981(3) .
Pd1B N3B 2.000(4) .
Pd1B C27B 2.019(4) .
Pd1B O1B 2.058(3) .
N1B N2B 1.279(4) .
N1B C15B 1.455(5) .
O1B C1B 1.277(4) .
C1B C6B 1.434(5) .
C1B C2B 1.436(5) .
N2B C2B 1.376(5) .
C2B C3B 1.426(5) .
N3B C28B 1.142(5) .
C3B C4B 1.358(5) .
C4B C5B 1.411(5) .
C4B C7B 1.528(5) .
C5B C6B 1.382(5) .
C6B C11B 1.534(5) .
C7B C10B 1.515(6) .
C7B C9B 1.516(6) .
C7B C8B 1.534(6) .
C11B C13B 1.524(6) .
C11B C14B 1.530(6) .
C11B C12B 1.538(6) .
C15B C20B 1.393(6) .
C15B C16B 1.405(6) .
C16B C17B 1.384(6) .
C16B C21B 1.515(7) .
C17B C18B 1.374(7) .
C18B C19B 1.369(7) .
C19B C20B 1.382(6) .
C20B C24B 1.505(6) .
C21B C22B 1.498(7) .
C21B C23B 1.538(7) .
C24B C25B 1.501(7) .
C24B C26B 1.508(7) .
C28B C29B 1.458(6) .
C1L C2L 1.36(8) .
C1L C3L 1.95(8) .
C2L C3L 1.05(7) .
C3L C3L 1.33(11) 2
C2L' C3L' 1.05(8) 2
C2L' C3L' 1.42(8) .
C3L' C2L' 1.05(8) 2
C3L' C3L' 1.15(8) 2
C2L" C3L" 1.12(7) .
C2L" C1L" 1.54(6) .
C3L" C1L" 1.45(8) .
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_4
C27 Pd1 N1 N2 -172.4(3) . .
O1 Pd1 N1 N2 11.4(3) . .
C27 Pd1 N1 C15 2.3(3) . .
O1 Pd1 N1 C15 -173.9(3) . .
N1 Pd1 O1 C1 -10.4(3) . .
N3 Pd1 O1 C1 165.1(3) . .
Pd1 O1 C1 C2 3.9(6) . .
Pd1 O1 C1 C6 -176.0(3) . .
C15 N1 N2 C2 178.7(3) . .
Pd1 N1 N2 C2 -6.0(5) . .
N1 N2 C2 C3 176.0(3) . .
N1 N2 C2 C1 -5.7(6) . .
O1 C1 C2 N2 6.6(6) . .
C6 C1 C2 N2 -173.4(3) . .
O1 C1 C2 C3 -175.3(4) . .
C6 C1 C2 C3 4.7(6) . .
N2 C2 C3 C4 178.3(3) . .
C1 C2 C3 C4 -0.1(6) . .
C2 C3 C4 C5 -4.0(6) . .
C2 C3 C4 C7 177.2(4) . .
C3 C4 C5 C6 3.6(6) . .
C7 C4 C5 C6 -177.6(4) . .
C4 C5 C6 C1 1.0(6) . .
C4 C5 C6 C11 -179.8(4) . .
O1 C1 C6 C5 175.0(4) . .
C2 C1 C6 C5 -5.0(5) . .
O1 C1 C6 C11 -4.3(6) . .
C2 C1 C6 C11 175.7(4) . .
C3 C4 C7 C9 117.3(5) . .
C5 C4 C7 C9 -61.4(6) . .
C3 C4 C7 C8 -5.2(6) . .
C5 C4 C7 C8 176.0(4) . .
C3 C4 C7 C10 -123.5(5) . .
C5 C4 C7 C10 57.8(6) . .
C5 C6 C11 C14 -117.1(4) . .
C1 C6 C11 C14 62.2(5) . .
C5 C6 C11 C12 2.7(6) . .
C1 C6 C11 C12 -178.1(4) . .
C5 C6 C11 C13 121.4(4) . .
C1 C6 C11 C13 -59.4(5) . .
N2 N1 C15 C16 92.6(4) . .
Pd1 N1 C15 C16 -82.9(4) . .
N2 N1 C15 C20 -88.5(5) . .
Pd1 N1 C15 C20 96.0(4) . .
C20 C15 C16 C17 0.2(6) . .
N1 C15 C16 C17 179.0(4) . .
C20 C15 C16 C21 176.8(4) . .
N1 C15 C16 C21 -4.4(6) . .
C15 C16 C17 C18 0.4(6) . .
C21 C16 C17 C18 -176.3(4) . .
C16 C17 C18 C19 -1.4(7) . .
C17 C18 C19 C20 1.8(8) . .
C18 C19 C20 C15 -1.2(8) . .
C18 C19 C20 C24 178.6(5) . .
C16 C15 C20 C19 0.2(7) . .
N1 C15 C20 C19 -178.7(4) . .
C16 C15 C20 C24 -179.7(5) . .
N1 C15 C20 C24 1.5(7) . .
C17 C16 C21 C23 70.6(5) . .
C15 C16 C21 C23 -106.0(5) . .
C17 C16 C21 C22 -53.2(5) . .
C15 C16 C21 C22 130.3(4) . .
C19 C20 C24 C25 68.9(7) . .
C15 C20 C24 C25 -111.2(5) . .
C19 C20 C24 C26 -52.8(7) . .
C15 C20 C24 C26 127.0(5) . .
C27B Pd1B N1B N2B -171.2(3) . .
O1B Pd1B N1B N2B 7.0(3) . .
C27B Pd1B N1B C15B 6.5(3) . .
O1B Pd1B N1B C15B -175.3(3) . .
N1B Pd1B O1B C1B -11.2(3) . .
N3B Pd1B O1B C1B 170.2(3) . .
Pd1B O1B C1B C6B -172.1(3) . .
Pd1B O1B C1B C2B 9.3(5) . .
C15B N1B N2B C2B -178.8(3) . .
Pd1B N1B N2B C2B -0.9(5) . .
N1B N2B C2B C3B 175.9(3) . .
N1B N2B C2B C1B -5.4(6) . .
O1B C1B C2B N2B 0.5(6) . .
C6B C1B C2B N2B -178.1(3) . .
O1B C1B C2B C3B 179.2(3) . .
C6B C1B C2B C3B 0.6(5) . .
N2B C2B C3B C4B -179.7(3) . .
C1B C2B C3B C4B 1.5(6) . .
C2B C3B C4B C5B -1.7(5) . .
C2B C3B C4B C7B 178.9(4) . .
C3B C4B C5B C6B -0.1(6) . .
C7B C4B C5B C6B 179.3(4) . .
C4B C5B C6B C1B 2.1(6) . .
C4B C5B C6B C11B -178.2(4) . .
O1B C1B C6B C5B 179.1(3) . .
C2B C1B C6B C5B -2.2(5) . .
O1B C1B C6B C11B -0.6(5) . .
C2B C1B C6B C11B 178.1(3) . .
C3B C4B C7B C10B 6.1(6) . .
C5B C4B C7B C10B -173.3(4) . .
C3B C4B C7B C9B -117.0(5) . .
C5B C4B C7B C9B 63.5(5) . .
C3B C4B C7B C8B 125.1(4) . .
C5B C4B C7B C8B -54.3(5) . .
C5B C6B C11B C13B -116.5(4) . .
C1B C6B C11B C13B 63.2(5) . .
C5B C6B C11B C14B 3.1(5) . .
C1B C6B C11B C14B -177.2(4) . .
C5B C6B C11B C12B 123.0(4) . .
C1B C6B C11B C12B -57.3(5) . .
N2B N1B C15B C20B 73.5(4) . .
Pd1B N1B C15B C20B -104.6(4) . .
N2B N1B C15B C16B -107.0(4) . .
Pd1B N1B C15B C16B 75.0(4) . .
C20B C15B C16B C17B -0.8(6) . .
N1B C15B C16B C17B 179.7(4) . .
C20B C15B C16B C21B -179.4(4) . .
N1B C15B C16B C21B 1.1(6) . .
C15B C16B C17B C18B 0.4(7) . .
C21B C16B C17B C18B 179.0(5) . .
C16B C17B C18B C19B -0.3(7) . .
C17B C18B C19B C20B 0.5(7) . .
C18B C19B C20B C15B -0.8(6) . .
C18B C19B C20B C24B 177.1(4) . .
C16B C15B C20B C19B 1.0(6) . .
N1B C15B C20B C19B -179.5(3) . .
C16B C15B C20B C24B -176.9(4) . .
N1B C15B C20B C24B 2.7(6) . .
C17B C16B C21B C22B -84.7(5) . .
C15B C16B C21B C22B 93.8(5) . .
C17B C16B C21B C23B 38.8(7) . .
C15B C16B C21B C23B -142.7(5) . .
C19B C20B C24B C25B -90.6(5) . .
C15B C20B C24B C25B 87.2(5) . .
C19B C20B C24B C26B 34.5(6) . .
C15B C20B C24B C26B -147.7(5) . .
C1L C2L C3L C3L 173(5) . 2
C3L' C2L' C3L' C2L' 0.000(6) 2 2
