#------------------------------------------------------------------------------
#$Date: 2021-12-08 11:29:37 +0100 (Wed 08 de Dec de 2021) $
#$Revision: 271270 $
#$URL: svn://www.crystallography.net/cod/cif/1/56/56/1565600.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_1565600
loop_
_publ_author_name
'Carroll, Hannah K.'
'Brown, Matthew L.'
'Yap, Vanessa C.'
'Magnuson, Justine R.'
'Reich, Noah A.J.'
'Macdonald, Alexander G.P.'
'Montgomery, Craig D.'
_publ_section_title
;
 Rapid interconversion of diastereomers of
 [PdCl{P(OC6H4NMe)2}{P(OC6H4NMe)OC6H4NHMe}]
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119239
_journal_paper_doi               10.1016/j.ica.2019.119239
_journal_volume                  501
_journal_year                    2020
_chemical_formula_moiety         'C28 H29 Cl N4 O4 P2 Pd'
_chemical_formula_sum            'C28 H29 Cl N4 O4 P2 Pd'
_chemical_formula_weight         689.34
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                97.753(5)
_cell_angle_beta                 112.821(5)
_cell_angle_gamma                95.185(5)
_cell_formula_units_Z            4
_cell_length_a                   13.4859(8)
_cell_length_b                   13.9193(8)
_cell_length_c                   16.7686(10)
_cell_measurement_reflns_used    7497
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.76
_cell_measurement_theta_min      2.909
_cell_volume                     2839.5(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2018.1-0'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics
;
ShelxLe (H\:ubschle, 2011), Olex2 (Dolomanov et al., 2009)'
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.1446
_diffrn_reflns_Laue_measured_fraction_full 0.878
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10938
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        67.201
_diffrn_reflns_theta_max         67.201
_diffrn_reflns_theta_min         2.909
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.557
_exptl_absorpt_correction_T_max  0.752818
_exptl_absorpt_correction_T_min  0.461690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 5 output contains 38763 reflections, 
Rint = 0.1024  for all   19590  observations and
 Rint = 0.0472  for all    2224  observations with I > 3sigma(I)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1:1 THF/hexanes'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.205
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         10938
_refine_ls_number_restraints     777
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1490
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1148P)²+13.6919P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.2381
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6492
_reflns_number_total             10938
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-501-119239.cif
_cod_data_source_block           1
_cod_database_code               1565600
_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   0.864
_shelx_estimated_absorpt_t_min   0.519
_exptl_absorpt_special_details
;
HKLF 5 dataset constructed from all observed data
Reflections merged according to point-group -1    
Single reflections that also occur in composites not omitted
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.186(15) 0.14(2) 0.16(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-H2
 0.87 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N7) \\sim
Ueq, Uanis(N1) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.002 and sigma
for terminal atoms of 0.003
Uanis(C48) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.003
Uanis(C42) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.003
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
6.a Ternary CH refined with riding coordinates:
 N6(H6)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C16(H16), C19(H19), C18(H18), C23(H23), C26(H26), C25(H25), C24(H24),
  C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53),
  C54(H54)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C56(H56A,
 H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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 0.36364(12) 0.60137(12) 0.34014(9) 0.0165(4) Uani 1 1 d . U . . .
N1 N 0.5591(15) 0.6047(14) 0.2629(10) 0.024(3) Uani 1 1 d . U . . .
C1 C 0.4745(17) 0.634(2) 0.1234(14) 0.031(5) Uani 1 1 d . U . . .
O1 O 0.3877(11) 0.6126(13) 0.1478(10) 0.029(3) Uani 1 1 d . U . . .
P1 P 0.4296(4) 0.5717(4) 0.2398(3) 0.0186(11) Uani 1 1 d . U . . .
Cl1 Cl 0.2968(5) 0.6225(4) 0.4495(3) 0.0242(12) Uani 1 1 d . U . . .
Pd2 Pd 0.97790(12) 0.33609(12) 0.34257(9) 0.0170(4) Uani 1 1 d . U . . .
Cl2 Cl 1.1558(4) 0.3600(4) 0.4511(3) 0.0246(12) Uani 1 1 d . U . . .
P2 P 0.4001(4) 0.7673(4) 0.3499(4) 0.0190(11) Uani 1 1 d . U . . .
N2 N 0.3339(12) 0.4433(12) 0.3387(9) 0.010(3) Uani 1 1 d D U . . .
H2 H 0.307(12) 0.441(13) 0.378(8) 0.012 Uiso 1 1 d DR . . . .
O2 O 0.4121(13) 0.4531(13) 0.2053(10) 0.027(3) Uani 1 1 d . U . . .
C2 C 0.4628(16) 0.6553(18) 0.0447(14) 0.033(5) Uani 1 1 d . U . . .
H2A H 0.393483 0.657540 0.000228 0.040 Uiso 1 1 calc R . . . .
C3 C 0.5611(18) 0.675(2) 0.0322(17) 0.050(6) Uani 1 1 d . U . . .
H3 H 0.557992 0.690796 -0.021838 0.060 Uiso 1 1 calc R . . . .
O3 O 0.2670(14) 0.7678(13) 0.2817(9) 0.025(3) Uani 1 1 d . U . . .
P3 P 0.8107(4) 0.3236(4) 0.2437(3) 0.0188(11) Uani 1 1 d . U . . .
N3 N 0.4415(15) 0.8164(15) 0.2797(12) 0.025(4) Uani 1 1 d . U . . .
O4 O 0.5325(14) 0.7603(15) 0.4196(11) 0.032(4) Uani 1 1 d . U . . .
P4 P 0.9502(4) 0.1745(4) 0.3534(3) 0.0182(11) Uani 1 1 d . U . . .
N4 N 0.3950(16) 0.8499(16) 0.4315(11) 0.024(3) Uani 1 1 d . U . . .
C4 C 0.6597(19) 0.670(2) 0.0973(17) 0.049(7) Uani 1 1 d . U . . .
H4 H 0.723550 0.681224 0.086475 0.059 Uiso 1 1 calc R . . . .
N6 N 1.0048(14) 0.4982(13) 0.3400(9) 0.016(3) Uani 1 1 d . U . . .
H6 H 1.084501 0.521397 0.375009 0.019 Uiso 1 1 calc R . . . .
O6 O 0.7950(11) 0.4250(12) 0.2063(10) 0.024(3) Uani 1 1 d . U . . .
C6 C 0.5734(16) 0.6250(18) 0.1889(13) 0.025(4) Uani 1 1 d . U . . .
C5 C 0.6696(19) 0.6497(19) 0.1768(15) 0.032(5) Uani 1 1 d . U . . .
H5 H 0.739185 0.652102 0.222835 0.038 Uiso 1 1 calc R . . . .
N5 N 0.7064(13) 0.3075(12) 0.2726(9) 0.018(3) Uani 1 1 d . U . . .
O5 O 0.7554(11) 0.2411(11) 0.1542(8) 0.023(2) Uani 1 1 d . U . . .
C8 C 0.3077(18) 0.4020(16) 0.1841(12) 0.021(4) Uani 1 1 d . U . . .
O8 O 1.0120(13) 0.1451(13) 0.2819(10) 0.027(3) Uani 1 1 d . U . . .
N8 N 0.8366(15) 0.0948(14) 0.2838(12) 0.022(3) Uani 1 1 d . U . . .
C7 C 0.6536(19) 0.6072(18) 0.3468(13) 0.030(4) Uani 1 1 d . U . . .
H7A H 0.695334 0.555330 0.338965 0.044 Uiso 1 1 calc GR . . . .
H7B H 0.627853 0.596867 0.392600 0.044 Uiso 1 1 calc GR . . . .
H7C H 0.700310 0.671233 0.364296 0.044 Uiso 1 1 calc GR . . . .
N7 N 1.0410(16) 0.1263(15) 0.4326(11) 0.022(3) Uani 1 1 d . U . . .
O7 O 0.8885(13) 0.2079(13) 0.4242(9) 0.022(3) Uani 1 1 d . U . . .
C9 C 0.248(2) 0.3526(19) 0.0984(13) 0.034(5) Uani 1 1 d . U . . .
H9 H 0.274994 0.358575 0.054507 0.041 Uiso 1 1 calc R . . . .
C10 C 0.150(2) 0.295(2) 0.0768(18) 0.048(8) Uani 1 1 d . U . . .
H10 H 0.107744 0.263447 0.017634 0.057 Uiso 1 1 calc R . . . .
C11 C 0.113(2) 0.284(2) 0.1401(15) 0.040(6) Uani 1 1 d . U . . .
H11 H 0.045580 0.244439 0.125348 0.048 Uiso 1 1 calc R . . . .
C12 C 0.1755(18) 0.3324(18) 0.2284(14) 0.029(5) Uani 1 1 d . U . . .
H12 H 0.149022 0.326058 0.272597 0.035 Uiso 1 1 calc R . . . .
C13 C 0.2756(16) 0.3887(15) 0.2492(12) 0.015(3) Uani 1 1 d . U . . .
C17 C 0.163(2) 0.859(2) 0.0790(18) 0.047(7) Uani 1 1 d . U . . .
H17 H 0.096299 0.868637 0.034591 0.056 Uiso 1 1 calc R . . . .
C16 C 0.159(2) 0.816(2) 0.1439(15) 0.036(5) Uani 1 1 d . U . . .
H16 H 0.091129 0.790260 0.143878 0.044 Uiso 1 1 calc R . . . .
C15 C 0.2550(19) 0.811(2) 0.2108(14) 0.029(4) Uani 1 1 d . U . . .
C14 C 0.4410(18) 0.4062(18) 0.3877(14) 0.024(4) Uani 1 1 d . U . . .
H14A H 0.427439 0.334569 0.380572 0.036 Uiso 1 1 calc GR . . . .
H14B H 0.470108 0.435407 0.450435 0.036 Uiso 1 1 calc GR . . . .
H14C H 0.493759 0.425053 0.363478 0.036 Uiso 1 1 calc GR . . . .
C19 C 0.359(2) 0.8748(18) 0.1376(15) 0.032(4) Uani 1 1 d . U . . .
H19 H 0.426840 0.890110 0.132948 0.038 Uiso 1 1 calc R . . . .
C18 C 0.261(2) 0.891(2) 0.0735(16) 0.040(5) Uani 1 1 d . U . . .
H18 H 0.261150 0.922587 0.026895 0.047 Uiso 1 1 calc R . . . .
C21 C 0.5506(19) 0.853(2) 0.2879(15) 0.032(5) Uani 1 1 d . U . . .
H21A H 0.566533 0.813245 0.242767 0.048 Uiso 1 1 calc GR . . . .
H21B H 0.604140 0.848804 0.346402 0.048 Uiso 1 1 calc GR . . . .
H21C H 0.554375 0.921563 0.280067 0.048 Uiso 1 1 calc GR . . . .
C20 C 0.354(2) 0.8369(18) 0.2057(15) 0.026(4) Uani 1 1 d . U . . .
C22 C 0.561(2) 0.8104(17) 0.5033(14) 0.023(4) Uani 1 1 d . U . . .
C23 C 0.657(2) 0.8098(17) 0.5767(15) 0.029(4) Uani 1 1 d . U . . .
H23 H 0.713356 0.775781 0.572367 0.034 Uiso 1 1 calc R . . . .
C26 C 0.495(2) 0.912(2) 0.5924(16) 0.035(5) Uani 1 1 d . U . . .
H26 H 0.437603 0.943169 0.598996 0.042 Uiso 1 1 calc R . . . .
C25 C 0.594(2) 0.918(2) 0.6641(17) 0.048(7) Uani 1 1 d . U . . .
H25 H 0.610378 0.962140 0.717690 0.058 Uiso 1 1 calc R . . . .
C24 C 0.665(2) 0.8623(18) 0.6564(15) 0.031(4) Uani 1 1 d . U . . .
H24 H 0.725766 0.857665 0.708374 0.037 Uiso 1 1 calc R . . . .
C28 C 0.306(2) 0.904(2) 0.4276(19) 0.039(6) Uani 1 1 d . U . . .
H28A H 0.331321 0.974646 0.437223 0.058 Uiso 1 1 calc GR . . . .
H28B H 0.281317 0.890502 0.473408 0.058 Uiso 1 1 calc GR . . . .
H28C H 0.245283 0.883648 0.369695 0.058 Uiso 1 1 calc GR . . . .
C27 C 0.481(2) 0.8601(19) 0.5126(14) 0.026(3) Uani 1 1 d . U . . .
C29 C 0.6470(16) 0.2084(17) 0.1378(12) 0.023(4) Uani 1 1 d . U . . .
C30 C 0.5757(17) 0.1368(19) 0.0676(14) 0.034(5) Uani 1 1 d . U . . .
H30 H 0.596787 0.109471 0.022587 0.041 Uiso 1 1 calc R . . . .
C31 C 0.4738(17) 0.1062(18) 0.0646(15) 0.035(5) Uani 1 1 d . U . . .
H31 H 0.424873 0.056151 0.017880 0.042 Uiso 1 1 calc R . . . .
C32 C 0.4409(15) 0.1498(17) 0.1319(14) 0.033(4) Uani 1 1 d . U . . .
H32 H 0.369554 0.131793 0.128561 0.040 Uiso 1 1 calc R . . . .
C33 C 0.5166(16) 0.2186(18) 0.2015(15) 0.031(5) Uani 1 1 d . U . . .
H33 H 0.496894 0.248632 0.246394 0.038 Uiso 1 1 calc R . . . .
C34 C 0.6194(15) 0.2436(16) 0.2062(12) 0.020(3) Uani 1 1 d . U . . .
C35 C 0.7054(17) 0.3403(18) 0.3573(12) 0.028(5) Uani 1 1 d . U . . .
H35A H 0.663669 0.394809 0.354189 0.043 Uiso 1 1 calc GR . . . .
H35B H 0.780262 0.362284 0.401064 0.043 Uiso 1 1 calc GR . . . .
H35C H 0.671506 0.286015 0.374530 0.043 Uiso 1 1 calc GR . . . .
C36 C 0.8733(16) 0.4748(16) 0.1867(13) 0.017(4) Uani 1 1 d . U . . .
C37 C 0.8494(18) 0.481(2) 0.0981(14) 0.036(6) Uani 1 1 d . U . . .
H37 H 0.779446 0.454132 0.053705 0.043 Uiso 1 1 calc R . . . .
C38 C 0.9280(19) 0.527(2) 0.0757(15) 0.037(6) Uani 1 1 d . U . . .
H38 H 0.911327 0.532762 0.016167 0.044 Uiso 1 1 calc R . . . .
C39 C 1.0337(18) 0.5666(18) 0.1418(14) 0.032(5) Uani 1 1 d . U . . .
H39 H 1.087482 0.598332 0.126619 0.039 Uiso 1 1 calc R . . . .
C40 C 1.0571(17) 0.5583(18) 0.2272(14) 0.025(4) Uani 1 1 d . U . . .
H40 H 1.127838 0.584827 0.270713 0.030 Uiso 1 1 calc R . . . .
C41 C 0.9831(16) 0.5134(16) 0.2523(13) 0.017(4) Uani 1 1 d . U . . .
C42 C 0.951(2) 0.5503(19) 0.3867(13) 0.026(4) Uani 1 1 d . U . . .
H42A H 0.919009 0.602540 0.356104 0.039 Uiso 1 1 calc GR . . . .
H42B H 1.003004 0.579108 0.446649 0.039 Uiso 1 1 calc GR . . . .
H42C H 0.892434 0.504716 0.389219 0.039 Uiso 1 1 calc GR . . . .
C43 C 0.9442(19) 0.1970(18) 0.5105(14) 0.023(4) Uani 1 1 d . U . . .
C44 C 0.920(2) 0.227(2) 0.5785(15) 0.031(4) Uani 1 1 d . U . . .
H44 H 0.858956 0.259199 0.571588 0.037 Uiso 1 1 calc R . . . .
C45 C 0.988(2) 0.2092(18) 0.6605(14) 0.029(4) Uani 1 1 d . U . . .
H45 H 0.974102 0.231043 0.710815 0.035 Uiso 1 1 calc R . . . .
C46 C 1.077(2) 0.1590(19) 0.6692(14) 0.032(5) Uani 1 1 d . U . . .
H46 H 1.121917 0.146193 0.725097 0.038 Uiso 1 1 calc R . . . .
C47 C 1.099(2) 0.1284(19) 0.5964(13) 0.027(3) Uani 1 1 d . U . . .
H47 H 1.158538 0.094342 0.602482 0.032 Uiso 1 1 calc R . . . .
C48 C 1.0347(18) 0.1469(17) 0.5160(12) 0.020(3) Uani 1 1 d . U . . .
C49 C 1.121(2) 0.063(2) 0.4289(16) 0.031(5) Uani 1 1 d . U . . .
H49A H 1.104941 0.036047 0.367337 0.047 Uiso 1 1 calc GR . . . .
H49B H 1.116317 0.008429 0.459777 0.047 Uiso 1 1 calc GR . . . .
H49C H 1.194194 0.100711 0.457205 0.047 Uiso 1 1 calc GR . . . .
C50 C 0.9497(17) 0.0733(17) 0.2120(14) 0.023(4) Uani 1 1 d . U . . .
C51 C 0.984(2) 0.0265(19) 0.1500(15) 0.033(5) Uani 1 1 d . U . . .
H51 H 1.054341 0.045751 0.152365 0.040 Uiso 1 1 calc R . . . .
C52 C 0.909(2) -0.051(2) 0.083(2) 0.045(6) Uani 1 1 d . U . . .
H52 H 0.928153 -0.081524 0.037725 0.054 Uiso 1 1 calc R . . . .
C53 C 0.810(2) -0.082(2) 0.084(2) 0.056(7) Uani 1 1 d . U . . .
H53 H 0.762429 -0.135513 0.040575 0.067 Uiso 1 1 calc R . . . .
C54 C 0.7759(19) -0.037(2) 0.1461(16) 0.040(5) Uani 1 1 d . U . . .
H54 H 0.707096 -0.060879 0.145341 0.048 Uiso 1 1 calc R . . . .
C55 C 0.8450(17) 0.0436(17) 0.2107(13) 0.023(4) Uani 1 1 d . U . . .
C56 C 0.7407(18) 0.066(2) 0.3010(15) 0.032(5) Uani 1 1 d . U . . .
H56A H 0.674608 0.063137 0.247669 0.049 Uiso 1 1 calc GR . . . .
H56B H 0.739691 0.114186 0.348857 0.049 Uiso 1 1 calc GR . . . .
H56C H 0.743458 0.001191 0.317839 0.049 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 0.0181 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
P1 Pd1 Cl1 176.0(2) . .
P1 Pd1 P2 91.9(2) . .
P2 Pd1 Cl1 91.7(2) . .
N2 Pd1 P1 90.0(4) . .
N2 Pd1 Cl1 86.4(4) . .
N2 Pd1 P2 176.8(4) . .
C6 N1 P1 110.7(13) . .
C6 N1 C7 121.1(18) . .
C7 N1 P1 128.0(15) . .
C2 C1 O1 124.2(19) . .
C2 C1 C6 124(2) . .
C6 C1 O1 111.6(18) . .
C1 O1 P1 110.4(13) . .
N1 P1 Pd1 121.3(6) . .
O1 P1 Pd1 124.0(6) . .
O1 P1 N1 94.2(8) . .
O1 P1 O2 102.0(9) . .
O2 P1 Pd1 109.6(6) . .
O2 P1 N1 102.4(9) . .
P3 Pd2 Cl2 176.3(2) . .
P3 Pd2 P4 91.3(2) . .
P3 Pd2 N6 89.7(4) . .
P4 Pd2 Cl2 91.9(2) . .
N6 Pd2 Cl2 87.0(4) . .
N6 Pd2 P4 176.5(4) . .
O3 P2 Pd1 90.1(6) . .
O3 P2 O4 176.8(10) . .
N3 P2 Pd1 122.3(8) . .
N3 P2 O3 90.1(9) . .
N3 P2 O4 92.2(9) . .
N3 P2 N4 114.6(11) . .
O4 P2 Pd1 86.8(7) . .
N4 P2 Pd1 122.9(8) . .
N4 P2 O3 92.9(9) . .
N4 P2 O4 88.1(9) . .
Pd1 N2 H2 103(10) . .
C13 N2 Pd1 111.1(12) . .
C13 N2 H2 121(10) . .
C13 N2 C14 112.2(16) . .
C14 N2 Pd1 110.6(12) . .
C14 N2 H2 98(10) . .
C8 O2 P1 115.9(14) . .
C1 C2 H2A 122.1 . .
C1 C2 C3 116(2) . .
C3 C2 H2A 122.1 . .
C2 C3 H3 119.6 . .
C4 C3 C2 121(2) . .
C4 C3 H3 119.6 . .
C15 O3 P2 113.8(15) . .
O6 P3 Pd2 109.3(6) . .
O6 P3 N5 102.0(9) . .
O6 P3 O5 102.4(8) . .
N5 P3 Pd2 119.9(6) . .
O5 P3 Pd2 124.9(6) . .
O5 P3 N5 94.9(8) . .
C21 N3 P2 130.8(16) . .
C20 N3 P2 113.3(16) . .
C20 N3 C21 115(2) . .
C22 O4 P2 112.5(15) . .
O8 P4 Pd2 89.4(6) . .
N8 P4 Pd2 123.0(7) . .
N8 P4 O8 89.5(8) . .
N8 P4 O7 91.3(9) . .
N7 P4 Pd2 122.0(8) . .
N7 P4 O8 91.9(9) . .
N7 P4 N8 115.1(10) . .
N7 P4 O7 89.3(8) . .
O7 P4 Pd2 88.7(6) . .
O7 P4 O8 178.1(9) . .
C28 N4 P2 127.3(17) . .
C27 N4 P2 115.7(17) . .
C27 N4 C28 117(2) . .
C3 C4 H4 118.8 . .
C5 C4 C3 122(2) . .
C5 C4 H4 118.8 . .
Pd2 N6 H6 105.9 . .
C41 N6 Pd2 110.5(13) . .
C41 N6 H6 105.9 . .
C41 N6 C42 117.8(17) . .
C42 N6 Pd2 109.9(14) . .
C42 N6 H6 105.9 . .
C36 O6 P3 122.2(14) . .
N1 C6 C1 110.5(18) . .
N1 C6 C5 130(2) . .
C1 C6 C5 118.6(19) . .
C4 C5 C6 118(2) . .
C4 C5 H5 121.1 . .
C6 C5 H5 121.1 . .
C34 N5 P3 110.5(12) . .
C34 N5 C35 121.4(17) . .
C35 N5 P3 127.5(14) . .
C29 O5 P3 110.0(12) . .
C9 C8 O2 118.5(19) . .
C13 C8 O2 119.4(17) . .
C13 C8 C9 121(2) . .
C50 O8 P4 113.0(14) . .
C55 N8 P4 114.8(15) . .
C55 N8 C56 118(2) . .
C56 N8 P4 126.2(16) . .
N1 C7 H7A 109.5 . .
N1 C7 H7B 109.5 . .
N1 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C48 N7 P4 114.1(16) . .
C48 N7 C49 114.9(18) . .
C49 N7 P4 131.0(15) . .
C43 O7 P4 115.6(14) . .
C8 C9 H9 119.9 . .
C10 C9 C8 120(2) . .
C10 C9 H9 119.9 . .
C9 C10 H10 120.2 . .
C11 C10 C9 120(2) . .
C11 C10 H10 120.2 . .
C10 C11 H11 119.8 . .
C10 C11 C12 120(2) . .
C12 C11 H11 119.8 . .
C11 C12 H12 120.5 . .
C13 C12 C11 119(2) . .
C13 C12 H12 120.5 . .
C8 C13 N2 122.2(18) . .
C8 C13 C12 119.2(19) . .
C12 C13 N2 117.9(18) . .
C16 C17 H17 118.9 . .
C16 C17 C18 122(2) . .
C18 C17 H17 118.9 . .
C17 C16 H16 121.1 . .
C17 C16 C15 118(3) . .
C15 C16 H16 121.1 . .
O3 C15 C20 112(2) . .
C16 C15 O3 126(2) . .
C16 C15 C20 121(2) . .
N2 C14 H14A 109.5 . .
N2 C14 H14B 109.5 . .
N2 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C18 C19 H19 121.4 . .
C20 C19 H19 121.4 . .
C20 C19 C18 117(2) . .
C17 C18 C19 119(2) . .
C17 C18 H18 120.3 . .
C19 C18 H18 120.3 . .
N3 C21 H21A 109.5 . .
N3 C21 H21B 109.5 . .
N3 C21 H21C 109.5 . .
H21A C21 H21B 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C15 C20 N3 110(2) . .
C19 C20 N3 128(2) . .
C19 C20 C15 121(2) . .
O4 C22 C23 126(2) . .
O4 C22 C27 113(2) . .
C27 C22 C23 120(2) . .
C22 C23 H23 122.1 . .
C24 C23 C22 116(2) . .
C24 C23 H23 122.1 . .
C25 C26 H26 120.7 . .
C27 C26 H26 120.7 . .
C27 C26 C25 119(3) . .
C26 C25 H25 120.5 . .
C24 C25 C26 119(2) . .
C24 C25 H25 120.5 . .
C23 C24 H24 118.0 . .
C25 C24 C23 124(2) . .
C25 C24 H24 118.0 . .
N4 C28 H28A 109.5 . .
N4 C28 H28B 109.5 . .
N4 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
N4 C27 C22 109(2) . .
C26 C27 N4 130(3) . .
C26 C27 C22 121(2) . .
C30 C29 O5 125.5(19) . .
C34 C29 O5 113.0(16) . .
C34 C29 C30 121(2) . .
C29 C30 H30 120.7 . .
C31 C30 C29 119(2) . .
C31 C30 H30 120.7 . .
C30 C31 H31 119.7 . .
C30 C31 C32 121(2) . .
C32 C31 H31 119.7 . .
C31 C32 H32 121.0 . .
C33 C32 C31 118.0(18) . .
C33 C32 H32 121.0 . .
C32 C33 H33 119.7 . .
C34 C33 C32 121(2) . .
C34 C33 H33 119.7 . .
C29 C34 N5 110.8(17) . .
C33 C34 N5 128.3(19) . .
C33 C34 C29 120.9(19) . .
N5 C35 H35A 109.5 . .
N5 C35 H35B 109.5 . .
N5 C35 H35C 109.5 . .
H35A C35 H35B 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
O6 C36 C37 118.6(17) . .
O6 C36 C41 122.8(17) . .
C37 C36 C41 118(2) . .
C36 C37 H37 120.0 . .
C38 C37 C36 120(2) . .
C38 C37 H37 120.0 . .
C37 C38 H38 119.9 . .
C37 C38 C39 120(2) . .
C39 C38 H38 119.9 . .
C38 C39 H39 120.2 . .
C40 C39 C38 120(2) . .
C40 C39 H39 120.2 . .
C39 C40 H40 118.7 . .
C41 C40 C39 123(2) . .
C41 C40 H40 118.7 . .
N6 C41 C36 115.7(18) . .
C40 C41 N6 124.9(18) . .
C40 C41 C36 119.4(19) . .
N6 C42 H42A 109.5 . .
N6 C42 H42B 109.5 . .
N6 C42 H42C 109.5 . .
H42A C42 H42B 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
O7 C43 C48 108.9(18) . .
C44 C43 O7 127(2) . .
C44 C43 C48 124(2) . .
C43 C44 H44 121.2 . .
C43 C44 C45 118(3) . .
C45 C44 H44 121.2 . .
C44 C45 H45 119.8 . .
C44 C45 C46 120(2) . .
C46 C45 H45 119.8 . .
C45 C46 H46 119.9 . .
C47 C46 C45 120(2) . .
C47 C46 H46 119.9 . .
C46 C47 H47 119.9 . .
C48 C47 C46 120(2) . .
C48 C47 H47 119.9 . .
N7 C48 C43 111.2(18) . .
C47 C48 N7 131(2) . .
C47 C48 C43 117(2) . .
N7 C49 H49A 109.5 . .
N7 C49 H49B 109.5 . .
N7 C49 H49C 109.5 . .
H49A C49 H49B 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
O8 C50 C51 125(2) . .
O8 C50 C55 112.7(19) . .
C51 C50 C55 122(2) . .
C50 C51 H51 120.9 . .
C50 C51 C52 118(2) . .
C52 C51 H51 120.9 . .
C51 C52 H52 120.1 . .
C53 C52 C51 120(3) . .
C53 C52 H52 120.1 . .
C52 C53 H53 118.7 . .
C52 C53 C54 123(2) . .
C54 C53 H53 118.7 . .
C53 C54 H54 120.4 . .
C53 C54 C55 119(2) . .
C55 C54 H54 120.4 . .
N8 C55 C50 109.8(19) . .
N8 C55 C54 131(2) . .
C54 C55 C50 118(2) . .
N8 C56 H56A 109.5 . .
N8 C56 H56B 109.5 . .
N8 C56 H56C 109.5 . .
H56A C56 H56B 109.5 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 P1 2.198(5) .
Pd1 Cl1 2.334(5) .
Pd1 P2 2.287(6) .
Pd1 N2 2.196(16) .
N1 P1 1.641(18) .
N1 C6 1.39(2) .
N1 C7 1.48(2) .
C1 O1 1.40(2) .
C1 C2 1.34(3) .
C1 C6 1.39(3) .
O1 P1 1.626(15) .
P1 O2 1.638(18) .
Pd2 Cl2 2.342(5) .
Pd2 P3 2.194(5) .
Pd2 P4 2.289(6) .
Pd2 N6 2.262(18) .
P2 O3 1.715(17) .
P2 N3 1.680(19) .
P2 O4 1.734(17) .
P2 N4 1.691(19) .
N2 H2 0.88(2) .
N2 C13 1.46(2) .
N2 C14 1.53(2) .
O2 C8 1.41(3) .
C2 H2A 0.9500 .
C2 C3 1.43(3) .
C3 H3 0.9500 .
C3 C4 1.37(3) .
O3 C15 1.37(3) .
P3 O6 1.618(16) .
P3 N5 1.662(17) .
P3 O5 1.625(14) .
N3 C21 1.46(3) .
N3 C20 1.43(3) .
O4 C22 1.37(3) .
P4 O8 1.733(16) .
P4 N8 1.701(19) .
P4 N7 1.685(19) .
P4 O7 1.733(15) .
N4 C28 1.46(3) .
N4 C27 1.38(3) .
C4 H4 0.9500 .
C4 C5 1.36(3) .
N6 H6 1.0000 .
N6 C41 1.43(2) .
N6 C42 1.44(3) .
O6 C36 1.38(3) .
C6 C5 1.41(3) .
C5 H5 0.9500 .
N5 C34 1.39(2) .
N5 C35 1.44(2) .
O5 C29 1.40(2) .
C8 C9 1.39(3) .
C8 C13 1.35(3) .
O8 C50 1.36(3) .
N8 C55 1.38(3) .
N8 C56 1.46(3) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
N7 C48 1.43(3) .
N7 C49 1.47(3) .
O7 C43 1.38(2) .
C9 H9 0.9500 .
C9 C10 1.37(4) .
C10 H10 0.9500 .
C10 C11 1.35(4) .
C11 H11 0.9500 .
C11 C12 1.42(3) .
C12 H12 0.9500 .
C12 C13 1.39(3) .
C17 H17 0.9500 .
C17 C16 1.32(3) .
C17 C18 1.40(3) .
C16 H16 0.9500 .
C16 C15 1.36(3) .
C15 C20 1.39(3) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C19 H19 0.9500 .
C19 C18 1.41(3) .
C19 C20 1.34(3) .
C18 H18 0.9500 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 C23 1.40(3) .
C22 C27 1.38(4) .
C23 H23 0.9500 .
C23 C24 1.39(3) .
C26 H26 0.9500 .
C26 C25 1.40(3) .
C26 C27 1.37(3) .
C25 H25 0.9500 .
C25 C24 1.32(4) .
C24 H24 0.9500 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 C30 1.39(3) .
C29 C34 1.38(3) .
C30 H30 0.9500 .
C30 C31 1.38(3) .
C31 H31 0.9500 .
C31 C32 1.45(3) .
C32 H32 0.9500 .
C32 C33 1.38(3) .
C33 H33 0.9500 .
C33 C34 1.37(3) .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C36 C37 1.41(3) .
C36 C41 1.46(2) .
C37 H37 0.9500 .
C37 C38 1.39(3) .
C38 H38 0.9500 .
C38 C39 1.42(3) .
C39 H39 0.9500 .
C39 C40 1.36(3) .
C40 H40 0.9500 .
C40 C41 1.36(3) .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 C44 1.33(3) .
C43 C48 1.44(3) .
C44 H44 0.9500 .
C44 C45 1.39(3) .
C45 H45 0.9500 .
C45 C46 1.41(3) .
C46 H46 0.9500 .
C46 C47 1.39(3) .
C47 H47 0.9500 .
C47 C48 1.36(3) .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C50 C51 1.40(3) .
C50 C55 1.42(3) .
C51 H51 0.9500 .
C51 C52 1.43(3) .
C52 H52 0.9500 .
C52 C53 1.38(4) .
C53 H53 0.9500 .
C53 C54 1.38(4) .
C54 H54 0.9500 .
C54 C55 1.42(3) .
C56 H56A 0.9800 .
C56 H56B 0.9800 .
C56 H56C 0.9800 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(3)
2 0.186(15)
3 0.14(2)
4 0.16(2)
