#------------------------------------------------------------------------------
#$Date: 2025-10-30 01:15:05 +0200 (Thu, 30 Oct 2025) $
#$Revision: 303095 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/61/1576120.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_1576120
loop_
_publ_author_name
'Zhang, Cheng'
'Leforestier, Baptiste'
'Besnard, Céline'
'Mazet, Clement'
_publ_section_title
;
 Pd-Catalyzed Regiodivergent Arylation of Cyclic Allylboronates
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC07577G
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H37 Br N P Pd'
_chemical_formula_sum            'C28 H37 Br N P Pd'
_chemical_formula_weight         604.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-25
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-24 deposited with the CCDC.	2025-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.12340(10)
_cell_length_b                   10.90100(10)
_cell_length_c                   51.1310(3)
_cell_measurement_reflns_used    122974
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      74.6540
_cell_measurement_theta_min      2.6020
_cell_volume                     5642.57(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  36.00   0.50    1.14    --    4.00  30.00 170.38   54
  2  ω     11.00  37.00   0.50    1.14    --    4.00  30.00  44.46   52
  3  ω      5.00  31.00   0.50    1.14    --   -4.00  33.00 -98.57   52
  4  ω      9.00  34.00   0.50    1.14    --    4.00  30.00   2.45   50
  5  ω      1.00  27.00   0.50    1.14    --   -8.00  35.00 -53.59   52
  6  ω      1.00  27.00   0.50    1.14    --   -8.00  35.00-152.33   52
  7  ω      1.00  27.00   0.50    1.14    --   -8.00  35.00 111.18   52
  8  ω     11.00  36.00   0.50    1.14    --    8.00  29.00-132.88   50
  9  ω     15.00  40.00   0.50    1.14    --   16.00  27.00  94.00   50
 10  ω     17.00  48.00   0.50    1.14    --   20.00  26.00 -65.26   62
 11  ω     17.00  45.00   0.50    1.14    --   20.00  26.00 134.43   56
 12  ω     -8.00  18.00   0.50    1.14    --  -20.00  42.00  12.79   52
 13  ω    -12.00  15.00   0.50    1.14    --  -24.00  45.00 122.48   54
 14  ω    -50.00 -24.00   0.50    1.14    --  -32.00 -25.00 -20.77   52
 15  ω    -51.00 -24.00   0.50    1.14    --  -32.00 -25.00-112.23   54
 16  ω    -51.00 -26.00   0.50    1.14    --  -32.00 -25.00-162.27   50
 17  ω     24.00  56.00   0.50    1.14    --   36.00  24.00-172.88   64
 18  ω    -30.00   2.00   0.50    1.14    --  -40.00  59.00-114.82   64
 19  ω    -30.00   2.00   0.50    1.14    --  -40.00  58.00 -37.69   64
 20  ω    -29.00   2.00   0.50    1.14    --  -40.00  59.00  25.13   62
 21  ω    -53.00 -28.00   0.50    1.14    --  -40.00 -24.00  83.94   50
 22  ω    -62.00 -34.00   0.50    1.14    --  -48.00 -23.00 173.05   56
 23  ω    -62.00 -37.00   0.50    1.14    --  -48.00 -23.00 135.68   50
 24  ω    -62.00 -37.00   0.50    1.14    --  -48.00 -23.00 -19.86   50
 25  ω     34.00  59.00   0.50    1.14    --   48.00  23.00-147.16   50
 26  ω    -62.00 -36.00   0.50    1.14    --  -48.00 -23.00 147.60   52
 27  ω    -62.00 -34.00   0.50    1.14    --  -48.00 -23.00 -56.70   56
 28  ω    -60.00 -34.00   0.50    1.14    --  -48.00 -23.00-133.75   52
 29  ω    -70.00 -45.00   0.50    1.14    --  -60.00 -22.00  83.13   50
 30  ω    -69.00 -44.00   0.50    1.14    --  -60.00 -22.00 119.70   50
 31  ω    -46.00 -20.00   0.50    1.14    --  -60.50  64.00   8.49   52
 32  ω    -47.00 -19.00   0.50    1.14    --  -60.50  56.00 104.08   56
 33  ω    -39.00 -14.00   0.50    1.14    --  -60.50  36.00-109.23   50
 34  ω    -38.00 -13.00   0.50    1.14    --  -60.50  36.00 -39.57   50
 35  ω    -40.00 -14.00   0.50    1.14    --  -60.50  37.00 -51.04   52
 36  ω    -39.00 -14.00   0.50    1.14    --  -60.50  36.00-154.40   50
 37  ω    -40.00 -15.00   0.50    1.14    --  -60.50  37.00-146.41   50
 38  ω    -40.00 -15.00   0.50    1.14    --  -60.50  37.00 158.24   50
 39  ω    -40.00 -14.00   0.50    1.14    --  -60.50  38.00  89.16   52
 40  ω    -52.00 -27.00   0.50    1.14    --  -60.50  63.00-145.16   50
 41  ω    -47.00 -19.00   0.50    1.14    --  -60.50  60.00 118.33   56
 42  ω    -39.00 -14.00   0.50    1.14    --  -60.50  36.00-179.27   50
 43  ω     31.00  70.00   0.50    1.14    --   64.48 -94.00 150.00   78
 44  ω     41.00  91.00   0.50    1.14    --   64.48-125.00 -90.00  100
 45  ω     49.00  90.00   0.50    1.14    --   64.48-125.00  60.00   82
 46  ω     58.00  91.00   0.50    1.14    --   64.48-125.00   0.00   66
 47  ω     59.00  88.00   0.50    1.14    --   70.96  21.00 -50.61   58
 48  ω     53.00  87.00   0.50    1.14    --   70.96  21.00  51.54   68
 49  ω     55.00 116.00   0.50    1.14    --   70.96  21.00  93.71  122
 50  ω     53.00 116.00   0.50    1.14    --   70.96  21.00 -16.00  126
 51  ω     53.00 103.00   0.50    1.14    --   70.96  21.00 152.58  100
 52  ω     92.00 117.00   0.50    1.14    --   70.96  21.00 -50.61   50
 53  ω     56.00  98.00   0.50    1.14    --   72.65-125.00 -30.00   84
 54  ω     35.00  98.00   0.50    1.14    --   72.65-125.00 120.00  126
 55  ω     44.00  80.00   0.50    1.14    --   72.65 -94.00-180.00   72
 56  ω     39.00  66.00   0.50    1.14    --   77.44-125.00  60.00   54
 57  ω     36.00 102.00   0.50    1.14    --   77.44-125.00 -30.00  132
 58  ω     36.00 104.00   0.50    1.14    --   77.44-125.00-120.00  136
 59  ω     79.00 104.00   0.50    1.14    --   77.44-125.00-180.00   50
 60  ω     36.00  75.00   0.50    1.14    --   77.44-125.00-180.00   78
 61  ω     36.00 104.00   0.50    1.14    --   77.44-125.00  30.00  136
 62  ω     40.00 102.00   0.50    1.14    --   77.44-125.00 -90.00  124
 63  ω     79.00 104.00   0.50    1.14    --   77.44-125.00  90.00   50
 64  ω     36.00  75.00   0.50    1.14    --   77.44-125.00  90.00   78
 65  ω     37.00 104.00   0.50    1.14    --   77.44-125.00 150.00  134
 66  ω     36.00 104.00   0.50    1.14    --   77.44-125.00 -60.00  136
 67  ω     79.00 104.00   0.50    1.14    --   77.44-125.00-150.00   50
 68  ω     36.00  72.00   0.50    1.14    --   77.44-125.00-150.00   72
 69  ω     36.00 104.00   0.50    1.14    --   77.44-125.00 120.00  136
 70  ω     69.00 103.00   0.50    1.14    --   77.44-125.00  60.00   68
 71  ω     37.00  78.00   0.50    1.14    --   77.50-125.00   4.53   82
 72  ω     77.00 106.00   0.50    1.14    --   77.50-126.00  -8.82   58
 73  ω     40.00  70.00   0.50    1.14    --   77.50-126.00  -8.82   60
 74  ω     56.00 119.00   0.50    1.14    --   77.50  20.00  18.48  126
 75  ω     56.00 117.00   0.50    1.14    --   77.50   3.00-143.58  122
 76  ω     43.00 119.00   0.50    1.14    --   77.50   6.00  17.31  152
 77  ω     62.00  88.00   0.50    1.14    --   77.50  22.00  52.04   52
 78  ω     48.00 102.00   0.50    1.14    --   77.50   3.00 162.61  108
 79  ω     92.00 118.00   0.50    1.14    --   77.50  22.00 -65.28   52
 80  ω     62.00  87.00   0.50    1.14    --   77.50  22.00 -65.28   50
 81  ω     62.00 113.00   0.50    1.14    --   77.50  22.00 158.15  102
 82  ω     62.00 124.00   0.50    1.14    --   77.50  22.00-151.73  124
 83  ω     42.00 117.00   0.50    1.14    --   77.50   3.00 -63.07  150
 84  ω     63.00  98.00   0.50    1.14    --   77.50  21.00  76.82   70
 85  ω     62.00 110.00   0.50    1.14    --   77.50  22.00 -43.68   96
 86  ω     62.00 108.00   0.50    1.14    --   77.50  22.00 113.04   92
 87  ω     62.00 107.00   0.50    1.14    --   77.50  22.00-110.51   90
 88  ω     42.00 116.00   0.50    1.14    --   77.50   3.00  96.51  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0569040000
_diffrn_orient_matrix_UB_12      -0.1310333000
_diffrn_orient_matrix_UB_13      0.0005832000
_diffrn_orient_matrix_UB_21      0.0397283000
_diffrn_orient_matrix_UB_22      -0.0174730000
_diffrn_orient_matrix_UB_23      -0.0288438000
_diffrn_orient_matrix_UB_31      0.1354807000
_diffrn_orient_matrix_UB_32      -0.0500012000
_diffrn_orient_matrix_UB_33      0.0086539000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            160153
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.910
_diffrn_reflns_theta_min         3.458
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.599
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.196
_refine_diff_density_max         1.422
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.

Two complexes with the same configuration are present in the unit cell.
;
_refine_ls_abs_structure_Flack   0.021(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0415
_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)+(0.0559P)²+10.5800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                11508
_reflns_number_total             11544
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc07577g2.cif
_cod_data_source_block           complex16
_cod_database_code               1576120
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'Au1 Cl1 C48 H56 N2'
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.979(10)
 0.021(10)
2. 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
3.a Ternary CH refined with riding coordinates:
 C11(H11), C11B(H11B)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C10B(H10C,H10D)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C17(H17), C18(H18), C21(H21),
 C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C2B(H2B), C3B(H3B), C4B(H4B),
  C5B(H5B), C6B(H6B), C17B(H17B), C18B(H18B), C21B(H21B), C22B(H22B),
 C24B(H24B), C25B(H25B), C27B(H27B), C28B(H28B)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F),
 C15B(H15D,H15E,H15F), C20B(H20D,H20E,H20F), C29B(H29D,H29E,H29F)
;
_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 2.375
_oxdiff_exptl_absorpt_empirical_full_min 0.548
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'
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 0.57713(5) 0.23513(4) 0.52309(2) 0.03263(11) Uani 1 1 d . . . . .
Br1 Br 0.58980(8) 0.06701(6) 0.49007(2) 0.03864(16) Uani 1 1 d . . . . .
P1 P 0.52072(17) 0.37692(16) 0.55139(3) 0.0340(3) Uani 1 1 d . . . . .
N7 N 0.5691(6) 0.3874(5) 0.49284(10) 0.0354(11) Uani 1 1 d . . . . .
C1 C 0.6040(8) 0.1157(7) 0.55247(13) 0.0419(15) Uani 1 1 d . . . . .
C2 C 0.7144(7) 0.1293(8) 0.56899(14) 0.0439(16) Uani 1 1 d . . . . .
H2 H 0.771034 0.198228 0.567051 0.053 Uiso 1 1 calc R U . . .
C3 C 0.7403(10) 0.0427(9) 0.58796(16) 0.060(2) Uani 1 1 d . . . . .
H3 H 0.816481 0.051475 0.598635 0.072 Uiso 1 1 calc R U . . .
C4 C 0.6582(13) -0.0557(9) 0.59173(17) 0.069(3) Uani 1 1 d . . . . .
H4 H 0.675800 -0.113684 0.605165 0.083 Uiso 1 1 calc R U . . .
C5 C 0.5498(13) -0.0692(8) 0.57568(18) 0.072(3) Uani 1 1 d . . . . .
H5 H 0.493278 -0.138053 0.577859 0.087 Uiso 1 1 calc R U . . .
C6 C 0.5218(10) 0.0174(7) 0.55619(16) 0.0533(19) Uani 1 1 d . . . . .
H6 H 0.445642 0.007897 0.545533 0.064 Uiso 1 1 calc R U . . .
C8 C 0.6989(7) 0.3782(7) 0.47971(14) 0.0398(14) Uani 1 1 d . . . . .
H8A H 0.769099 0.397729 0.492224 0.060 Uiso 1 1 calc R U . . .
H8B H 0.702183 0.436253 0.465083 0.060 Uiso 1 1 calc R U . . .
H8C H 0.711326 0.294608 0.473107 0.060 Uiso 1 1 calc R U . . .
C9 C 0.4631(7) 0.3611(7) 0.47358(14) 0.0418(15) Uani 1 1 d . . . . .
H9A H 0.467160 0.274625 0.468437 0.063 Uiso 1 1 calc R U . . .
H9B H 0.475352 0.413001 0.458111 0.063 Uiso 1 1 calc R U . . .
H9C H 0.376903 0.378502 0.481468 0.063 Uiso 1 1 calc R U . . .
C10 C 0.4512(6) 0.4895(6) 0.52893(13) 0.0359(14) Uani 1 1 d . . . . .
H10A H 0.366530 0.459090 0.521739 0.043 Uiso 1 1 calc R U . . .
H10B H 0.434311 0.567559 0.538226 0.043 Uiso 1 1 calc R U . . .
C11 C 0.5510(6) 0.5100(6) 0.50672(13) 0.0362(14) Uani 1 1 d . . . . .
H11 H 0.637130 0.525522 0.515706 0.043 Uiso 1 1 calc R U . . .
C12 C 0.5196(8) 0.6326(7) 0.49155(16) 0.0462(17) Uani 1 1 d . . . . .
C13 C 0.5357(9) 0.7368(7) 0.51147(19) 0.058(2) Uani 1 1 d . . . . .
H13A H 0.462594 0.734265 0.524016 0.087 Uiso 1 1 calc R U . . .
H13B H 0.535323 0.815769 0.502330 0.087 Uiso 1 1 calc R U . . .
H13C H 0.619631 0.726777 0.520796 0.087 Uiso 1 1 calc R U . . .
C14 C 0.3798(9) 0.6412(7) 0.48032(18) 0.055(2) Uani 1 1 d . . . . .
H14A H 0.371759 0.585971 0.465283 0.083 Uiso 1 1 calc R U . . .
H14B H 0.362423 0.725684 0.474714 0.083 Uiso 1 1 calc R U . . .
H14C H 0.315632 0.617579 0.493756 0.083 Uiso 1 1 calc R U . . .
C15 C 0.6212(9) 0.6553(8) 0.46985(17) 0.055(2) Uani 1 1 d . . . . .
H15A H 0.710200 0.639409 0.476602 0.082 Uiso 1 1 calc R U . . .
H15B H 0.615172 0.740636 0.463959 0.082 Uiso 1 1 calc R U . . .
H15C H 0.603286 0.600249 0.455112 0.082 Uiso 1 1 calc R U . . .
C16 C 0.3945(7) 0.3475(6) 0.57608(13) 0.0380(14) Uani 1 1 d . . . . .
C17 C 0.2661(7) 0.3869(8) 0.57253(14) 0.0447(16) Uani 1 1 d . . . . .
H17 H 0.242789 0.430057 0.557057 0.054 Uiso 1 1 calc R U . . .
C18 C 0.1708(8) 0.3638(8) 0.59144(15) 0.0490(18) Uani 1 1 d . . . . .
H18 H 0.083110 0.392197 0.588712 0.059 Uiso 1 1 calc R U . . .
C19 C 0.2002(8) 0.3009(7) 0.61404(15) 0.0451(16) Uani 1 1 d . . . . .
C20 C 0.0970(9) 0.2829(9) 0.63509(17) 0.060(2) Uani 1 1 d . . . . .
H20A H 0.067860 0.363085 0.641579 0.091 Uiso 1 1 calc R U . . .
H20B H 0.134930 0.235494 0.649536 0.091 Uiso 1 1 calc R U . . .
H20C H 0.021255 0.238587 0.627796 0.091 Uiso 1 1 calc R U . . .
C21 C 0.3296(8) 0.2590(8) 0.61731(15) 0.0483(17) Uani 1 1 d . . . . .
H21 H 0.351887 0.213792 0.632565 0.058 Uiso 1 1 calc R U . . .
C22 C 0.4264(8) 0.2822(7) 0.59865(14) 0.0457(16) Uani 1 1 d . . . . .
H22 H 0.514003 0.253644 0.601280 0.055 Uiso 1 1 calc R U . . .
C23 C 0.6523(7) 0.4594(6) 0.56789(13) 0.0362(14) Uani 1 1 d . . . . .
C24 C 0.7798(7) 0.4607(7) 0.55703(13) 0.0391(14) Uani 1 1 d . . . . .
H24 H 0.799243 0.409037 0.542569 0.047 Uiso 1 1 calc R U . . .
C25 C 0.8766(7) 0.5353(7) 0.56693(14) 0.0423(15) Uani 1 1 d . . . . .
H25 H 0.962142 0.534438 0.559303 0.051 Uiso 1 1 calc R U . . .
C26 C 0.8509(7) 0.6124(7) 0.58806(13) 0.0406(15) Uani 1 1 d . . . . .
C27 C 0.7248(8) 0.6114(7) 0.59888(14) 0.0437(16) Uani 1 1 d . . . . .
H27 H 0.705387 0.663195 0.613318 0.052 Uiso 1 1 calc R U . . .
C28 C 0.6277(7) 0.5362(6) 0.58891(13) 0.0400(15) Uani 1 1 d . . . . .
H28 H 0.542292 0.537024 0.596603 0.048 Uiso 1 1 calc R U . . .
C29 C 0.9580(9) 0.6955(9) 0.59892(18) 0.060(2) Uani 1 1 d . . . . .
H29A H 0.923619 0.779209 0.600548 0.090 Uiso 1 1 calc R U . . .
H29B H 1.034014 0.695312 0.587059 0.090 Uiso 1 1 calc R U . . .
H29C H 0.985424 0.665663 0.616164 0.090 Uiso 1 1 calc R U . . .
Pd1B Pd 0.57396(5) 0.75736(4) 0.70979(2) 0.03532(12) Uani 1 1 d . . . . .
Br1B Br 0.37778(8) 0.88875(9) 0.71992(2) 0.0525(2) Uani 1 1 d . . . . .
P1B P 0.74718(17) 0.64374(15) 0.70041(3) 0.0343(3) Uani 1 1 d . . . . .
N7B N 0.6949(6) 0.8100(5) 0.74632(11) 0.0354(12) Uani 1 1 d . . . . .
C1B C 0.4833(7) 0.6901(7) 0.67816(14) 0.0379(14) Uani 1 1 d . . . . .
C2B C 0.4784(7) 0.7521(8) 0.65463(13) 0.0430(15) Uani 1 1 d . . . . .
H2B H 0.520511 0.829574 0.652928 0.052 Uiso 1 1 calc R U . . .
C3B C 0.4113(8) 0.7008(8) 0.63317(14) 0.0504(18) Uani 1 1 d . . . . .
H3B H 0.408383 0.744229 0.617068 0.060 Uiso 1 1 calc R U . . .
C4B C 0.3507(8) 0.5902(8) 0.63514(15) 0.0513(19) Uani 1 1 d . . . . .
H4B H 0.305665 0.556497 0.620505 0.062 Uiso 1 1 calc R U . . .
C5B C 0.3546(8) 0.5266(8) 0.65851(16) 0.0484(17) Uani 1 1 d . . . . .
H5B H 0.312816 0.448870 0.659947 0.058 Uiso 1 1 calc R U . . .
C6B C 0.4199(7) 0.5766(7) 0.67991(14) 0.0434(15) Uani 1 1 d . . . . .
H6B H 0.421418 0.532908 0.695983 0.052 Uiso 1 1 calc R U . . .
C8B C 0.6979(9) 0.9466(7) 0.74596(16) 0.0506(18) Uani 1 1 d . . . . .
H8BA H 0.747712 0.974702 0.730663 0.076 Uiso 1 1 calc R U . . .
H8BB H 0.740521 0.976663 0.761927 0.076 Uiso 1 1 calc R U . . .
H8BC H 0.607383 0.978188 0.745055 0.076 Uiso 1 1 calc R U . . .
C9B C 0.6118(7) 0.7651(8) 0.76813(13) 0.0456(16) Uani 1 1 d . . . . .
H9BA H 0.522217 0.798026 0.766312 0.068 Uiso 1 1 calc R U . . .
H9BB H 0.649630 0.792182 0.784796 0.068 Uiso 1 1 calc R U . . .
H9BC H 0.608598 0.675249 0.767705 0.068 Uiso 1 1 calc R U . . .
C10B C 0.8185(7) 0.6264(6) 0.73281(12) 0.0349(13) Uani 1 1 d . . . . .
H10C H 0.761099 0.573584 0.743724 0.042 Uiso 1 1 calc R U . . .
H10D H 0.906455 0.587116 0.731512 0.042 Uiso 1 1 calc R U . . .
C11B C 0.8315(6) 0.7532(7) 0.74528(12) 0.0362(13) Uani 1 1 d . . . . .
H11B H 0.881832 0.803512 0.732309 0.043 Uiso 1 1 calc R U . . .
C12B C 0.9222(7) 0.7473(7) 0.77027(13) 0.0415(14) Uani 1 1 d . . . . .
C13B C 1.0627(7) 0.7325(9) 0.76001(17) 0.058(2) Uani 1 1 d . . . . .
H13D H 1.083639 0.800541 0.748199 0.087 Uiso 1 1 calc R U . . .
H13E H 1.070060 0.654682 0.750518 0.087 Uiso 1 1 calc R U . . .
H13F H 1.124727 0.732643 0.774729 0.087 Uiso 1 1 calc R U . . .
C14B C 0.8912(9) 0.6395(8) 0.78845(16) 0.053(2) Uani 1 1 d . . . . .
H14D H 0.951450 0.641207 0.803455 0.080 Uiso 1 1 calc R U . . .
H14E H 0.902468 0.562278 0.778911 0.080 Uiso 1 1 calc R U . . .
H14F H 0.799860 0.646123 0.794639 0.080 Uiso 1 1 calc R U . . .
C15B C 0.9213(9) 0.8660(7) 0.78640(14) 0.0467(16) Uani 1 1 d . . . . .
H15D H 0.935651 0.936298 0.774801 0.070 Uiso 1 1 calc R U . . .
H15E H 0.991753 0.862798 0.799513 0.070 Uiso 1 1 calc R U . . .
H15F H 0.835713 0.874631 0.795179 0.070 Uiso 1 1 calc R U . . .
C16B C 0.7305(7) 0.4904(7) 0.68711(12) 0.0374(14) Uani 1 1 d . . . . .
C17B C 0.6849(7) 0.3971(7) 0.70267(13) 0.0396(15) Uani 1 1 d . . . . .
H17B H 0.671270 0.410788 0.720819 0.047 Uiso 1 1 calc R U . . .
C18B C 0.6585(7) 0.2826(7) 0.69195(14) 0.0422(16) Uani 1 1 d . . . . .
H18B H 0.627724 0.218635 0.702995 0.051 Uiso 1 1 calc R U . . .
C19B C 0.6760(7) 0.2597(7) 0.66560(13) 0.0430(16) Uani 1 1 d . . . . .
C20B C 0.6426(10) 0.1343(7) 0.65478(17) 0.056(2) Uani 1 1 d . . . . .
H20D H 0.724366 0.090220 0.650639 0.084 Uiso 1 1 calc R U . . .
H20E H 0.589571 0.143463 0.638870 0.084 Uiso 1 1 calc R U . . .
H20F H 0.592300 0.087878 0.667834 0.084 Uiso 1 1 calc R U . . .
C21B C 0.7242(9) 0.3528(8) 0.65040(14) 0.0505(19) Uani 1 1 d . . . . .
H21B H 0.737697 0.338486 0.632273 0.061 Uiso 1 1 calc R U . . .
C22B C 0.7542(8) 0.4681(7) 0.66067(13) 0.0459(17) Uani 1 1 d . . . . .
H22B H 0.790124 0.530464 0.649813 0.055 Uiso 1 1 calc R U . . .
C23B C 0.8726(7) 0.7243(6) 0.68190(12) 0.0367(14) Uani 1 1 d . . . . .
C24B C 0.8420(8) 0.8366(7) 0.67056(15) 0.0440(16) Uani 1 1 d . . . . .
H24B H 0.753368 0.865273 0.670569 0.053 Uiso 1 1 calc R U . . .
C25B C 0.9414(9) 0.9073(7) 0.65916(17) 0.0527(19) Uani 1 1 d . . . . .
H25B H 0.918933 0.983203 0.651180 0.063 Uiso 1 1 calc R U . . .
C26B C 1.0722(8) 0.8695(7) 0.65921(14) 0.0438(15) Uani 1 1 d . . . . .
C27B C 1.1025(7) 0.7567(8) 0.67070(14) 0.0454(15) Uani 1 1 d . . . . .
H27B H 1.191492 0.729172 0.670995 0.054 Uiso 1 1 calc R U . . .
C28B C 1.0052(7) 0.6851(7) 0.68158(14) 0.0419(16) Uani 1 1 d . . . . .
H28B H 1.027731 0.608008 0.688993 0.050 Uiso 1 1 calc R U . . .
C29B C 1.1793(9) 0.9470(9) 0.6476(2) 0.062(2) Uani 1 1 d . . . . .
H29D H 1.211100 0.908877 0.631397 0.093 Uiso 1 1 calc R U . . .
H29E H 1.252534 0.954026 0.660027 0.093 Uiso 1 1 calc R U . . .
H29F H 1.144481 1.028895 0.643682 0.093 Uiso 1 1 calc R U . . .
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'
Br Br -0.6763 1.2805 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0992
0 0 -1 0.1277
2 -1 -1 0.1001
-2 1 1 0.0959
0 1 0 0.1115
0 -1 0 0.0996
0 -1 -1 0.0894
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 Br1 167.85(5) . . ?
P1 Pd1 N7 85.69(15) . . ?
N7 Pd1 Br1 94.46(14) . . ?
C1 Pd1 Br1 91.3(2) . . ?
C1 Pd1 P1 89.9(2) . . ?
C1 Pd1 N7 171.6(3) . . ?
C10 P1 Pd1 99.2(2) . . ?
C10 P1 C16 106.5(3) . . ?
C16 P1 Pd1 121.0(2) . . ?
C23 P1 Pd1 117.7(2) . . ?
C23 P1 C10 104.1(3) . . ?
C23 P1 C16 106.2(3) . . ?
C8 N7 Pd1 103.2(4) . . ?
C8 N7 C9 109.1(5) . . ?
C8 N7 C11 112.1(5) . . ?
C9 N7 Pd1 109.7(4) . . ?
C9 N7 C11 113.0(5) . . ?
C11 N7 Pd1 109.2(4) . . ?
C2 C1 Pd1 119.2(6) . . ?
C6 C1 Pd1 121.9(6) . . ?
C6 C1 C2 118.8(7) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(8) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.3(9) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.6 . . ?
C3 C4 C5 118.8(8) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.8(9) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 120.2(9) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7 C9 H9A 109.5 . . ?
N7 C9 H9B 109.5 . . ?
N7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P1 C10 H10A 110.1 . . ?
P1 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C11 C10 P1 108.1(4) . . ?
C11 C10 H10A 110.1 . . ?
C11 C10 H10B 110.1 . . ?
N7 C11 C10 107.2(5) . . ?
N7 C11 H11 105.0 . . ?
N7 C11 C12 122.6(6) . . ?
C10 C11 H11 105.0 . . ?
C10 C11 C12 110.7(6) . . ?
C12 C11 H11 105.0 . . ?
C13 C12 C11 106.2(6) . . ?
C14 C12 C11 115.0(6) . . ?
C14 C12 C13 107.6(7) . . ?
C14 C12 C15 109.8(7) . . ?
C15 C12 C11 110.9(6) . . ?
C15 C12 C13 106.8(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 P1 120.9(5) . . ?
C17 C16 C22 119.0(7) . . ?
C22 C16 P1 120.1(6) . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.4(7) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 119.2 . . ?
C19 C18 C17 121.6(7) . . ?
C19 C18 H18 119.2 . . ?
C18 C19 C20 120.8(7) . . ?
C18 C19 C21 117.8(7) . . ?
C21 C19 C20 121.4(7) . . ?
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 . . ?
C19 C21 H21 119.4 . . ?
C22 C21 C19 121.3(7) . . ?
C22 C21 H21 119.4 . . ?
C16 C22 H22 120.1 . . ?
C21 C22 C16 119.9(7) . . ?
C21 C22 H22 120.1 . . ?
C24 C23 P1 119.7(5) . . ?
C28 C23 P1 121.9(5) . . ?
C28 C23 C24 117.7(7) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 C23 121.1(6) . . ?
C25 C24 H24 119.4 . . ?
C24 C25 H25 119.6 . . ?
C24 C25 C26 120.7(7) . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C29 120.7(7) . . ?
C27 C26 C25 118.4(7) . . ?
C27 C26 C29 121.0(7) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.8(7) . . ?
C28 C27 H27 119.6 . . ?
C23 C28 H28 119.4 . . ?
C27 C28 C23 121.3(7) . . ?
C27 C28 H28 119.4 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
P1B Pd1B Br1B 179.15(6) . . ?
P1B Pd1B N7B 83.90(15) . . ?
N7B Pd1B Br1B 96.38(14) . . ?
C1B Pd1B Br1B 90.76(19) . . ?
C1B Pd1B P1B 89.0(2) . . ?
C1B Pd1B N7B 172.1(2) . . ?
C10B P1B Pd1B 100.2(2) . . ?
C16B P1B Pd1B 121.8(2) . . ?
C16B P1B C10B 106.4(3) . . ?
C23B P1B Pd1B 113.6(2) . . ?
C23B P1B C10B 104.4(3) . . ?
C23B P1B C16B 108.5(3) . . ?
C8B N7B Pd1B 104.5(5) . . ?
C8B N7B C11B 112.9(6) . . ?
C9B N7B Pd1B 103.1(4) . . ?
C9B N7B C8B 110.6(6) . . ?
C9B N7B C11B 114.2(5) . . ?
C11B N7B Pd1B 110.7(4) . . ?
C2B C1B Pd1B 122.8(6) . . ?
C2B C1B C6B 118.2(7) . . ?
C6B C1B Pd1B 119.0(5) . . ?
C1B C2B H2B 119.9 . . ?
C1B C2B C3B 120.2(8) . . ?
C3B C2B H2B 119.9 . . ?
C2B C3B H3B 119.5 . . ?
C4B C3B C2B 120.9(7) . . ?
C4B C3B H3B 119.5 . . ?
C3B C4B H4B 120.1 . . ?
C3B C4B C5B 119.8(7) . . ?
C5B C4B H4B 120.1 . . ?
C4B C5B H5B 120.1 . . ?
C4B C5B C6B 119.9(8) . . ?
C6B C5B H5B 120.1 . . ?
C1B C6B H6B 119.5 . . ?
C5B C6B C1B 121.0(7) . . ?
C5B C6B H6B 119.5 . . ?
N7B C8B H8BA 109.5 . . ?
N7B C8B H8BB 109.5 . . ?
N7B C8B H8BC 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
N7B C9B H9BA 109.5 . . ?
N7B C9B H9BB 109.5 . . ?
N7B C9B H9BC 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
P1B C10B H10C 110.0 . . ?
P1B C10B H10D 110.0 . . ?
H10C C10B H10D 108.3 . . ?
C11B C10B P1B 108.7(4) . . ?
C11B C10B H10C 110.0 . . ?
C11B C10B H10D 110.0 . . ?
N7B C11B C10B 107.8(5) . . ?
N7B C11B H11B 105.3 . . ?
N7B C11B C12B 121.3(5) . . ?
C10B C11B H11B 105.3 . . ?
C10B C11B C12B 110.6(6) . . ?
C12B C11B H11B 105.3 . . ?
C13B C12B C11B 105.6(5) . . ?
C13B C12B C14B 108.6(7) . . ?
C13B C12B C15B 106.3(6) . . ?
C14B C12B C11B 113.8(6) . . ?
C14B C12B C15B 108.6(6) . . ?
C15B C12B C11B 113.5(6) . . ?
C12B C13B H13D 109.5 . . ?
C12B C13B H13E 109.5 . . ?
C12B C13B H13F 109.5 . . ?
H13D C13B H13E 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C12B C14B H14D 109.5 . . ?
C12B C14B H14E 109.5 . . ?
C12B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C12B C15B H15D 109.5 . . ?
C12B C15B H15E 109.5 . . ?
C12B C15B H15F 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C17B C16B P1B 119.8(5) . . ?
C17B C16B C22B 119.4(7) . . ?
C22B C16B P1B 120.6(6) . . ?
C16B C17B H17B 119.9 . . ?
C16B C17B C18B 120.1(6) . . ?
C18B C17B H17B 119.9 . . ?
C17B C18B H18B 119.2 . . ?
C19B C18B C17B 121.5(7) . . ?
C19B C18B H18B 119.2 . . ?
C18B C19B C20B 119.4(8) . . ?
C21B C19B C18B 117.7(7) . . ?
C21B C19B C20B 122.8(7) . . ?
C19B C20B H20D 109.5 . . ?
C19B C20B H20E 109.5 . . ?
C19B C20B H20F 109.5 . . ?
H20D C20B H20E 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C19B C21B H21B 118.9 . . ?
C19B C21B C22B 122.1(7) . . ?
C22B C21B H21B 118.9 . . ?
C16B C22B C21B 119.0(7) . . ?
C16B C22B H22B 120.5 . . ?
C21B C22B H22B 120.5 . . ?
C24B C23B P1B 119.3(5) . . ?
C24B C23B C28B 118.3(7) . . ?
C28B C23B P1B 121.8(5) . . ?
C23B C24B H24B 120.0 . . ?
C23B C24B C25B 120.0(7) . . ?
C25B C24B H24B 120.0 . . ?
C24B C25B H25B 119.2 . . ?
C26B C25B C24B 121.6(7) . . ?
C26B C25B H25B 119.2 . . ?
C25B C26B C27B 118.2(7) . . ?
C25B C26B C29B 121.5(7) . . ?
C27B C26B C29B 120.3(7) . . ?
C26B C27B H27B 119.6 . . ?
C28B C27B C26B 120.8(7) . . ?
C28B C27B H27B 119.6 . . ?
C23B C28B H28B 119.5 . . ?
C27B C28B C23B 121.0(7) . . ?
C27B C28B H28B 119.5 . . ?
C26B C29B H29D 109.5 . . ?
C26B C29B H29E 109.5 . . ?
C26B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
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 Br1 2.4951(8) . ?
Pd1 P1 2.1928(17) . ?
Pd1 N7 2.270(5) . ?
Pd1 C1 2.007(7) . ?
P1 C10 1.821(7) . ?
P1 C16 1.825(7) . ?
P1 C23 1.815(7) . ?
N7 C8 1.479(8) . ?
N7 C9 1.484(9) . ?
N7 C11 1.524(9) . ?
C1 C2 1.408(11) . ?
C1 C6 1.370(11) . ?
C2 H2 0.9500 . ?
C2 C3 1.379(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.379(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.401(12) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.536(9) . ?
C11 H11 1.0000 . ?
C11 C12 1.578(9) . ?
C12 C13 1.534(12) . ?
C12 C14 1.530(11) . ?
C12 C15 1.534(11) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.382(10) . ?
C16 C22 1.393(10) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.377(11) . ?
C19 C20 1.513(10) . ?
C19 C21 1.397(11) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 0.9500 . ?
C21 C22 1.391(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.406(10) . ?
C23 C28 1.385(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.370(10) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(10) . ?
C26 C27 1.391(11) . ?
C26 C29 1.518(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.377(11) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
Pd1B Br1B 2.5028(9) . ?
Pd1B P1B 2.1998(17) . ?
Pd1B N7B 2.306(6) . ?
Pd1B C1B 1.999(7) . ?
P1B C10B 1.817(7) . ?
P1B C16B 1.812(8) . ?
P1B C23B 1.810(7) . ?
N7B C8B 1.489(9) . ?
N7B C9B 1.480(9) . ?
N7B C11B 1.517(8) . ?
C1B C2B 1.381(10) . ?
C1B C6B 1.397(10) . ?
C2B H2B 0.9500 . ?
C2B C3B 1.406(11) . ?
C3B H3B 0.9500 . ?
C3B C4B 1.357(12) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.382(12) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.390(11) . ?
C6B H6B 0.9500 . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C10B C11B 1.528(9) . ?
C11B H11B 1.0000 . ?
C11B C12B 1.575(9) . ?
C12B C13B 1.524(10) . ?
C12B C14B 1.531(10) . ?
C12B C15B 1.534(10) . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C16B C17B 1.372(10) . ?
C16B C22B 1.394(9) . ?
C17B H17B 0.9500 . ?
C17B C18B 1.388(10) . ?
C18B H18B 0.9500 . ?
C18B C19B 1.382(10) . ?
C19B C20B 1.513(11) . ?
C19B C21B 1.368(12) . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C21B H21B 0.9500 . ?
C21B C22B 1.396(11) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.390(10) . ?
C23B C28B 1.409(10) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.395(11) . ?
C25B H25B 0.9500 . ?
C25B C26B 1.387(12) . ?
C26B C27B 1.397(11) . ?
C26B C29B 1.498(11) . ?
C27B H27B 0.9500 . ?
C27B C28B 1.374(10) . ?
C28B H28B 0.9500 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 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
_geom_torsion_publ_flag
Pd1 P1 C10 C11 -49.8(5) . . . . ?
Pd1 P1 C16 C17 -98.9(6) . . . . ?
Pd1 P1 C16 C22 79.8(6) . . . . ?
Pd1 P1 C23 C24 20.0(6) . . . . ?
Pd1 P1 C23 C28 -169.6(5) . . . . ?
Pd1 N7 C11 C10 -40.8(6) . . . . ?
Pd1 N7 C11 C12 -170.4(5) . . . . ?
Pd1 C1 C2 C3 -174.9(6) . . . . ?
Pd1 C1 C6 C5 175.0(7) . . . . ?
P1 C10 C11 N7 61.4(6) . . . . ?
P1 C10 C11 C12 -162.6(5) . . . . ?
P1 C16 C17 C18 179.9(6) . . . . ?
P1 C16 C22 C21 -179.4(6) . . . . ?
P1 C23 C24 C25 171.0(6) . . . . ?
P1 C23 C28 C27 -170.7(6) . . . . ?
N7 C11 C12 C13 -169.2(6) . . . . ?
N7 C11 C12 C14 71.8(9) . . . . ?
N7 C11 C12 C15 -53.5(9) . . . . ?
C1 C2 C3 C4 -1.9(12) . . . . ?
C2 C1 C6 C5 -1.6(12) . . . . ?
C2 C3 C4 C5 1.7(14) . . . . ?
C3 C4 C5 C6 -1.4(15) . . . . ?
C4 C5 C6 C1 1.4(15) . . . . ?
C6 C1 C2 C3 1.9(11) . . . . ?
C8 N7 C11 C10 -154.5(5) . . . . ?
C8 N7 C11 C12 75.9(8) . . . . ?
C9 N7 C11 C10 81.6(6) . . . . ?
C9 N7 C11 C12 -47.9(8) . . . . ?
C10 P1 C16 C17 13.0(7) . . . . ?
C10 P1 C16 C22 -168.4(6) . . . . ?
C10 P1 C23 C24 -88.5(6) . . . . ?
C10 P1 C23 C28 81.9(6) . . . . ?
C10 C11 C12 C13 62.7(7) . . . . ?
C10 C11 C12 C14 -56.2(9) . . . . ?
C10 C11 C12 C15 178.4(6) . . . . ?
C16 P1 C10 C11 -176.1(4) . . . . ?
C16 P1 C23 C24 159.3(6) . . . . ?
C16 P1 C23 C28 -30.3(7) . . . . ?
C16 C17 C18 C19 -0.5(13) . . . . ?
C17 C16 C22 C21 -0.8(11) . . . . ?
C17 C18 C19 C20 176.5(8) . . . . ?
C17 C18 C19 C21 -0.8(13) . . . . ?
C18 C19 C21 C22 1.3(12) . . . . ?
C19 C21 C22 C16 -0.6(12) . . . . ?
C20 C19 C21 C22 -176.0(8) . . . . ?
C22 C16 C17 C18 1.3(12) . . . . ?
C23 P1 C10 C11 71.9(5) . . . . ?
C23 P1 C16 C17 123.5(6) . . . . ?
C23 P1 C16 C22 -57.9(7) . . . . ?
C23 C24 C25 C26 -0.2(11) . . . . ?
C24 C23 C28 C27 0.0(10) . . . . ?
C24 C25 C26 C27 0.2(11) . . . . ?
C24 C25 C26 C29 -179.6(7) . . . . ?
C25 C26 C27 C28 -0.1(11) . . . . ?
C26 C27 C28 C23 0.0(11) . . . . ?
C28 C23 C24 C25 0.1(10) . . . . ?
C29 C26 C27 C28 179.7(7) . . . . ?
Pd1B P1B C10B C11B -50.9(5) . . . . ?
Pd1B P1B C16B C17B -71.0(6) . . . . ?
Pd1B P1B C16B C22B 104.1(6) . . . . ?
Pd1B P1B C23B C24B -13.2(6) . . . . ?
Pd1B P1B C23B C28B 158.0(5) . . . . ?
Pd1B N7B C11B C10B -36.3(6) . . . . ?
Pd1B N7B C11B C12B -165.3(5) . . . . ?
Pd1B C1B C2B C3B -179.0(5) . . . . ?
Pd1B C1B C6B C5B 179.4(6) . . . . ?
P1B C10B C11B N7B 58.5(6) . . . . ?
P1B C10B C11B C12B -166.7(4) . . . . ?
P1B C16B C17B C18B 173.1(6) . . . . ?
P1B C16B C22B C21B -171.9(6) . . . . ?
P1B C23B C24B C25B 171.7(6) . . . . ?
P1B C23B C28B C27B -170.3(6) . . . . ?
N7B C11B C12B C13B -158.7(7) . . . . ?
N7B C11B C12B C14B 82.3(8) . . . . ?
N7B C11B C12B C15B -42.6(9) . . . . ?
C1B C2B C3B C4B -0.1(12) . . . . ?
C2B C1B C6B C5B 0.6(10) . . . . ?
C2B C3B C4B C5B 0.0(12) . . . . ?
C3B C4B C5B C6B 0.4(12) . . . . ?
C4B C5B C6B C1B -0.7(11) . . . . ?
C6B C1B C2B C3B -0.2(10) . . . . ?
C8B N7B C11B C10B -153.1(6) . . . . ?
C8B N7B C11B C12B 78.0(8) . . . . ?
C9B N7B C11B C10B 79.4(7) . . . . ?
C9B N7B C11B C12B -49.5(8) . . . . ?
C10B P1B C16B C17B 42.5(6) . . . . ?
C10B P1B C16B C22B -142.3(6) . . . . ?
C10B P1B C23B C24B -121.3(6) . . . . ?
C10B P1B C23B C28B 49.9(7) . . . . ?
C10B C11B C12B C13B 73.6(7) . . . . ?
C10B C11B C12B C14B -45.4(8) . . . . ?
C10B C11B C12B C15B -170.3(6) . . . . ?
C16B P1B C10B C11B -178.6(4) . . . . ?
C16B P1B C23B C24B 125.5(6) . . . . ?
C16B P1B C23B C28B -63.3(7) . . . . ?
C16B C17B C18B C19B -0.6(11) . . . . ?
C17B C16B C22B C21B 3.3(11) . . . . ?
C17B C18B C19B C20B -178.5(7) . . . . ?
C17B C18B C19B C21B 1.9(11) . . . . ?
C18B C19B C21B C22B -0.6(12) . . . . ?
C19B C21B C22B C16B -2.0(12) . . . . ?
C20B C19B C21B C22B 179.8(8) . . . . ?
C22B C16B C17B C18B -2.1(11) . . . . ?
C23B P1B C10B C11B 66.8(5) . . . . ?
C23B P1B C16B C17B 154.3(6) . . . . ?
C23B P1B C16B C22B -30.5(7) . . . . ?
C23B C24B C25B C26B -1.2(13) . . . . ?
C24B C23B C28B C27B 1.0(11) . . . . ?
C24B C25B C26B C27B 1.0(12) . . . . ?
C24B C25B C26B C29B -178.4(8) . . . . ?
C25B C26B C27B C28B 0.2(11) . . . . ?
C26B C27B C28B C23B -1.2(12) . . . . ?
C28B C23B C24B C25B 0.2(11) . . . . ?
C29B C26B C27B C28B 179.6(8) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.979(10)
2 0.021(10)
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 -0.0001 0.9993 0.0006 -0.0288 0.0086
0.0000 0.0001 -0.9993 -0.0006 0.0288 -0.0086
1.9991 -0.9992 -0.9996 0.0166 0.1257 0.3121
-1.9991 0.9992 0.9996 -0.0166 -0.1257 -0.3121
-0.0001 0.9994 0.0004 -0.1309 -0.0175 -0.0500
0.0001 -0.9994 -0.0004 0.1309 0.0175 0.0500
0.0001 -0.9993 -0.9997 0.1304 0.0463 0.0413
