#------------------------------------------------------------------------------
#$Date: 2019-07-13 03:19:52 +0300 (Sat, 13 Jul 2019) $
#$Revision: 216988 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/20/1552098.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_1552098
loop_
_publ_author_name
'Scott, Neil W. J.'
'Ford, Mark J.'
'Schotes, Christoph'
'Parker, Rachel R.'
'Whitwood, Adrian C.'
'Fairlamb, Ian J. S.'
_publ_section_title
;
 The ubiquitous cross-coupling catalyst system
 ‘Pd(OAc)2’/2PPh3 forms a unique dinuclear PdI complex: an
 important entry point into catalytically competent cyclic Pd3 clusters
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01847F
_journal_year                    2019
_chemical_formula_moiety         'C54 H45 P3 Pd, 1.61(C3 H7), 0.39(C4 H8 O)'
_chemical_formula_sum            'C60.39 H59.39 O0.39 P3 Pd'
_chemical_formula_weight         990.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.    2019-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                92.507(2)
_cell_angle_beta                 111.038(2)
_cell_angle_gamma                96.346(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5043(4)
_cell_length_b                   13.6723(4)
_cell_length_c                   14.3402(4)
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      28.6610
_cell_measurement_theta_min      3.4890
_cell_volume                     2446.12(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      5.00  91.00   1.00   16.00    --   18.24  37.00  60.00   86
  2  ω     -7.00  89.00   1.00   16.00    --   18.24  37.00 150.00   96
  3  ω    -19.00  20.00   1.00   16.00    --   18.24 -99.00 -90.00   39
  4  ω    -17.00  60.00   1.00   16.00    --   18.24 -99.00 -30.00   77
  5  ω    -82.00  11.00   1.00   16.00    --  -18.55 -77.00-180.00   93
  6  ω     -1.00  25.00   1.00   16.00    --  -18.55  57.00  60.00   26
  7  ω    -93.00 -68.00   1.00   16.00    --  -18.55 154.00   6.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072445000
_diffrn_orient_matrix_UB_12      -0.0505953000
_diffrn_orient_matrix_UB_13      0.0009490000
_diffrn_orient_matrix_UB_21      0.0492362000
_diffrn_orient_matrix_UB_22      0.0122526000
_diffrn_orient_matrix_UB_23      0.0411197000
_diffrn_orient_matrix_UB_31      -0.0273735000
_diffrn_orient_matrix_UB_32      -0.0060736000
_diffrn_orient_matrix_UB_33      0.0337579000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20381
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.267
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             1031.7
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         9977
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0326
_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)+(0.0159P)²+1.8801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8672
_reflns_number_total             9977
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc01847f2.cif
_cod_data_source_block           ijsf1821
_cod_database_code               1552098
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C76 H66 O4 P4 Pd1'
_chemical_oxdiff_usercomment     'Neil Scott NWJS-4-293-crystals1'
_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.
;
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C61-O1 = C64-O1
 1.42 with sigma of 0.02
 C61-C62 = C62-C63 = C63-C64
 1.5 with sigma of 0.02
 C60-C59
 1.513 with sigma of 0.02
 C59-C58
 1.524 with sigma of 0.02
 C60-C58
 2.48 with sigma of 0.04
 C59-C58
 2.49 with sigma of 0.04
 C61-C64
 2.32 with sigma of 0.04
 C61-C63 = C62-C64
 2.36 with sigma of 0.04
 C62-O1 = C63-O1
 2.34 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C63) = Uanis(C62)
4. Others
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(O1)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C61)=
 Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=1-FVAR(1)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=
 Sof(H59A)=Sof(H59B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C56(H56A,H56B), C63(H63A,H63B), C60(H60A,H60B), C64(H64A,
 H64B), C61(H61A,H61B), C59(H59A,H59B), C62(H62A,H62B)
5.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C38(H38), C50(H50), C18(H18), C32(H32), C2(H2), C54(H54), C30(H30),
 C6(H6), C36(H36), C48(H48), C53(H53), C20(H20), C14(H14), C52(H52), C44(H44),
 C5(H5), C12(H12), C9(H9), C3(H3), C51(H51), C35(H35), C29(H29), C27(H27),
 C34(H34), C24(H24), C17(H17), C8(H8), C42(H42), C21(H21), C45(H45), C10(H10),
 C40(H40), C4(H4), C22(H22), C39(H39), C41(H41), C33(H33), C11(H11), C28(H28),
 C47(H47), C15(H15), C23(H23), C46(H46), C16(H16)
5.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C58(H58A,H58B,H58C)
;
_olex2_date_sample_data_collection 2018-10-19
_olex2_date_sample_submission    2018-10-19
_olex2_exptl_crystal_mounting_method 'oil on micrount 200 micrometres'
_olex2_submission_original_sample_id 'Neil Scott NWJS-4-293-crystals1'
_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 1.153
_oxdiff_exptl_absorpt_empirical_full_min 0.904
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.32139(2) 0.37183(2) 0.75551(2) 0.01302(5) Uani 1 1 d . . . .
P3 P 0.30886(4) 0.53910(4) 0.75540(4) 0.01329(12) Uani 1 1 d . . . .
P2 P 0.47747(5) 0.32832(4) 0.74322(4) 0.01345(12) Uani 1 1 d . . . .
P1 P 0.18184(5) 0.24640(4) 0.72682(4) 0.01395(12) Uani 1 1 d . . . .
C25 C 0.46402(18) 0.29665(16) 0.61288(16) 0.0152(5) Uani 1 1 d . . . .
C37 C 0.26400(17) 0.57649(16) 0.62695(16) 0.0155(5) Uani 1 1 d . . . .
C49 C 0.21666(17) 0.59474(16) 0.80424(16) 0.0141(4) Uani 1 1 d . . . .
C26 C 0.36149(18) 0.26835(16) 0.54249(17) 0.0174(5) Uani 1 1 d . . . .
H26 H 0.303070 0.265874 0.562589 0.021 Uiso 1 1 calc R . . .
C31 C 0.59901(17) 0.41892(16) 0.78728(16) 0.0142(4) Uani 1 1 d . . . .
C19 C 0.52957(18) 0.22091(16) 0.80788(16) 0.0157(5) Uani 1 1 d . . . .
C13 C 0.10811(17) 0.23089(17) 0.59006(16) 0.0154(5) Uani 1 1 d . . . .
C1 C 0.07185(18) 0.25568(16) 0.77298(16) 0.0162(5) Uani 1 1 d . . . .
C38 C 0.28120(19) 0.51784(17) 0.55353(17) 0.0202(5) Uani 1 1 d . . . .
H38 H 0.318869 0.464347 0.571556 0.024 Uiso 1 1 calc R . . .
C50 C 0.11002(18) 0.55051(17) 0.76935(17) 0.0187(5) Uani 1 1 d . . . .
H50 H 0.087773 0.496217 0.721837 0.022 Uiso 1 1 calc R . . .
C18 C 0.09863(18) 0.31695(17) 0.54044(17) 0.0189(5) Uani 1 1 d . . . .
H18 H 0.126509 0.377909 0.577281 0.023 Uiso 1 1 calc R . . .
C32 C 0.68249(18) 0.41305(17) 0.87724(17) 0.0191(5) Uani 1 1 d . . . .
H32 H 0.679698 0.359033 0.913876 0.023 Uiso 1 1 calc R . . .
C2 C 0.08533(19) 0.32727(17) 0.84960(17) 0.0204(5) Uani 1 1 d . . . .
H2 H 0.149793 0.369106 0.877479 0.024 Uiso 1 1 calc R . . .
C54 C 0.24809(18) 0.67479(16) 0.87652(16) 0.0169(5) Uani 1 1 d . . . .
H54 H 0.319009 0.704426 0.901467 0.020 Uiso 1 1 calc R . . .
C30 C 0.55034(18) 0.30112(17) 0.58056(17) 0.0184(5) Uani 1 1 d . . . .
H30 H 0.619505 0.320676 0.626440 0.022 Uiso 1 1 calc R . . .
C6 C -0.02579(18) 0.19416(18) 0.73222(17) 0.0202(5) Uani 1 1 d . . . .
H6 H -0.036385 0.146135 0.680358 0.024 Uiso 1 1 calc R . . .
C36 C 0.60529(19) 0.50165(17) 0.73437(17) 0.0186(5) Uani 1 1 d . . . .
H36 H 0.549560 0.508057 0.674708 0.022 Uiso 1 1 calc R . . .
C48 C 0.50655(18) 0.58833(18) 0.90499(17) 0.0195(5) Uani 1 1 d . . . .
H48 H 0.492195 0.524942 0.922144 0.023 Uiso 1 1 calc R . . .
C7 C 0.21099(18) 0.11992(16) 0.75398(16) 0.0164(5) Uani 1 1 d . . . .
C43 C 0.43348(17) 0.62213(16) 0.82102(16) 0.0151(5) Uani 1 1 d . . . .
C53 C 0.17461(19) 0.71103(17) 0.91193(17) 0.0188(5) Uani 1 1 d . . . .
H53 H 0.196441 0.764991 0.959805 0.023 Uiso 1 1 calc R . . .
C20 C 0.50457(19) 0.19951(17) 0.89129(17) 0.0210(5) Uani 1 1 d . . . .
H20 H 0.461245 0.237779 0.910666 0.025 Uiso 1 1 calc R . . .
C14 C 0.0652(2) 0.14112(18) 0.53325(18) 0.0247(5) Uani 1 1 d . . . .
H14 H 0.071024 0.082775 0.564638 0.030 Uiso 1 1 calc R . . .
C52 C 0.06916(19) 0.66694(18) 0.87604(17) 0.0212(5) Uani 1 1 d . . . .
H52 H 0.020080 0.691169 0.899730 0.025 Uiso 1 1 calc R . . .
C44 C 0.45771(19) 0.71634(17) 0.79524(17) 0.0196(5) Uani 1 1 d . . . .
H44 H 0.410018 0.739917 0.739001 0.023 Uiso 1 1 calc R . . .
C5 C -0.10684(19) 0.20365(18) 0.76786(18) 0.0241(5) Uani 1 1 d . . . .
H5 H -0.171283 0.161743 0.740317 0.029 Uiso 1 1 calc R . . .
C12 C 0.17188(19) 0.06241(18) 0.81417(17) 0.0218(5) Uani 1 1 d . . . .
H12 H 0.125376 0.086613 0.841268 0.026 Uiso 1 1 calc R . . .
C9 C 0.3108(2) -0.01143(18) 0.73592(19) 0.0263(6) Uani 1 1 d . . . .
H9 H 0.357685 -0.035917 0.709423 0.032 Uiso 1 1 calc R . . .
C3 C 0.0035(2) 0.33720(19) 0.88521(18) 0.0245(5) Uani 1 1 d . . . .
H3 H 0.013481 0.385606 0.936560 0.029 Uiso 1 1 calc R . . .
C51 C 0.03696(18) 0.58687(18) 0.80495(17) 0.0211(5) Uani 1 1 d . . . .
H51 H -0.033918 0.557159 0.780808 0.025 Uiso 1 1 calc R . . .
C35 C 0.69342(19) 0.57390(17) 0.76985(18) 0.0210(5) Uani 1 1 d . . . .
H35 H 0.697223 0.627706 0.733206 0.025 Uiso 1 1 calc R . . .
C29 C 0.5340(2) 0.27675(18) 0.48094(17) 0.0221(5) Uani 1 1 d . . . .
H29 H 0.591972 0.279953 0.460204 0.027 Uiso 1 1 calc R . . .
C27 C 0.34495(19) 0.24374(18) 0.44268(17) 0.0222(5) Uani 1 1 d . . . .
H27 H 0.275875 0.224668 0.396420 0.027 Uiso 1 1 calc R . . .
C34 C 0.77600(19) 0.56655(18) 0.85963(18) 0.0226(5) Uani 1 1 d . . . .
H34 H 0.835085 0.615334 0.883465 0.027 Uiso 1 1 calc R . . .
C24 C 0.5934(2) 0.16211(18) 0.77984(18) 0.0244(6) Uani 1 1 d . . . .
H24 H 0.611000 0.175470 0.724225 0.029 Uiso 1 1 calc R . . .
C17 C 0.04851(19) 0.31303(18) 0.43750(17) 0.0229(5) Uani 1 1 d . . . .
H17 H 0.043873 0.371083 0.405631 0.027 Uiso 1 1 calc R . . .
C8 C 0.28187(19) 0.08142(17) 0.71607(18) 0.0216(5) Uani 1 1 d . . . .
H8 H 0.310109 0.119014 0.676699 0.026 Uiso 1 1 calc R . . .
C42 C 0.20965(18) 0.65793(18) 0.59776(18) 0.0211(5) Uani 1 1 d . . . .
H42 H 0.198597 0.698772 0.645681 0.025 Uiso 1 1 calc R . . .
C21 C 0.5436(2) 0.12144(18) 0.94620(18) 0.0243(5) Uani 1 1 d . . . .
H21 H 0.527130 0.108323 1.002435 0.029 Uiso 1 1 calc R . . .
C45 C 0.5526(2) 0.77540(18) 0.85292(19) 0.0263(6) Uani 1 1 d . . . .
H45 H 0.568682 0.837885 0.834661 0.032 Uiso 1 1 calc R . . .
C10 C 0.2705(2) -0.06813(19) 0.79500(19) 0.0286(6) Uani 1 1 d . . . .
H10 H 0.289703 -0.130800 0.808190 0.034 Uiso 1 1 calc R . . .
C40 C 0.18766(19) 0.6184(2) 0.42624(18) 0.0273(6) Uani 1 1 d . . . .
H40 H 0.161201 0.631613 0.359301 0.033 Uiso 1 1 calc R . . .
C4 C -0.0926(2) 0.27538(19) 0.84454(18) 0.0243(5) Uani 1 1 d . . . .
H4 H -0.147316 0.281870 0.868458 0.029 Uiso 1 1 calc R . . .
C22 C 0.6065(2) 0.06379(18) 0.91731(18) 0.0256(6) Uani 1 1 d . . . .
H22 H 0.632411 0.011448 0.953792 0.031 Uiso 1 1 calc R . . .
C39 C 0.2427(2) 0.53852(19) 0.45401(18) 0.0248(6) Uani 1 1 d . . . .
H39 H 0.254017 0.498425 0.405696 0.030 Uiso 1 1 calc R . . .
C41 C 0.17207(19) 0.6785(2) 0.49820(18) 0.0260(6) Uani 1 1 d . . . .
H41 H 0.136202 0.733012 0.479823 0.031 Uiso 1 1 calc R . . .
C33 C 0.77011(19) 0.48648(18) 0.91345(18) 0.0238(5) Uani 1 1 d . . . .
H33 H 0.824969 0.481615 0.974204 0.029 Uiso 1 1 calc R . . .
C11 C 0.2016(2) -0.03064(19) 0.83413(19) 0.0282(6) Uani 1 1 d . . . .
H11 H 0.174669 -0.068201 0.874400 0.034 Uiso 1 1 calc R . . .
C28 C 0.4312(2) 0.24758(18) 0.41209(17) 0.0238(5) Uani 1 1 d . . . .
H28 H 0.420255 0.230601 0.345284 0.029 Uiso 1 1 calc R . . .
C47 C 0.60052(19) 0.6478(2) 0.96351(18) 0.0263(6) Uani 1 1 d . . . .
H47 H 0.648090 0.624693 1.020151 0.032 Uiso 1 1 calc R . . .
C15 C 0.0136(2) 0.1375(2) 0.42998(19) 0.0312(6) Uani 1 1 d . . . .
H15 H -0.015582 0.076862 0.392887 0.037 Uiso 1 1 calc R . . .
C23 C 0.6313(2) 0.08370(19) 0.83385(19) 0.0304(6) Uani 1 1 d . . . .
H23 H 0.673414 0.044376 0.813960 0.036 Uiso 1 1 calc R . . .
C46 C 0.6233(2) 0.7413(2) 0.93756(19) 0.0298(6) Uani 1 1 d . . . .
H46 H 0.686159 0.781447 0.976894 0.036 Uiso 1 1 calc R . . .
C16 C 0.0053(2) 0.22337(19) 0.38174(18) 0.0263(6) Uani 1 1 d . . . .
H16 H -0.029087 0.220686 0.312499 0.032 Uiso 1 1 calc R . . .
C57 C 0.4521(2) 1.0017(2) 0.5152(2) 0.0327(6) Uani 1 1 d . . . .
H57A H 0.456329 0.956700 0.566484 0.039 Uiso 1 1 calc R . . .
H57B H 0.455164 1.067846 0.544460 0.039 Uiso 1 1 calc R . . .
C56 C 0.3460(2) 0.9749(2) 0.4297(2) 0.0397(7) Uani 1 1 d . . . .
H56A H 0.341401 0.907586 0.402613 0.048 Uiso 1 1 calc R . . .
H56B H 0.343281 1.017766 0.376871 0.048 Uiso 1 1 calc R . . .
C55 C 0.2493(2) 0.9835(2) 0.4594(2) 0.0464(8) Uani 1 1 d . . . .
H55A H 0.245162 0.934265 0.504034 0.070 Uiso 1 1 calc GR . . .
H55B H 0.185192 0.973618 0.400358 0.070 Uiso 1 1 calc GR . . .
H55C H 0.256665 1.047985 0.492366 0.070 Uiso 1 1 calc GR . . .
C63 C 0.1665(8) 0.0646(8) 0.0780(7) 0.047(2) Uani 0.391(4) 1 d D P A 2
H63A H 0.229293 0.082194 0.061200 0.056 Uiso 0.391(4) 1 calc R P A 2
H63B H 0.143949 -0.006024 0.063735 0.056 Uiso 0.391(4) 1 calc R P A 2
O1 O 0.0147(4) 0.1281(4) 0.0842(3) 0.0350(15) Uani 0.391(4) 1 d D P A 2
C60 C 0.0260(4) 0.0238(4) 0.0532(3) 0.0360(12) Uani 0.609(4) 1 d D P A 1
H60A H -0.026322 0.056699 0.069930 0.043 Uiso 0.609(4) 1 calc R P A 1
H60B H 0.045896 -0.027628 0.098206 0.043 Uiso 0.609(4) 1 calc R P A 1
C64 C 0.0767(6) 0.1231(6) 0.0241(6) 0.036(2) Uani 0.391(4) 1 d D P A 2
H64A H 0.105587 0.188951 0.015912 0.043 Uiso 0.391(4) 1 calc R P A 2
H64B H 0.033510 0.090325 -0.041708 0.043 Uiso 0.391(4) 1 calc R P A 2
C61 C 0.0841(6) 0.1291(6) 0.1864(5) 0.041(2) Uani 0.391(4) 1 d D P A 2
H61A H 0.052190 0.083396 0.220892 0.049 Uiso 0.391(4) 1 calc R P A 2
H61B H 0.096461 0.194739 0.220265 0.049 Uiso 0.391(4) 1 calc R P A 2
C58 C 0.1702(5) 0.1465(4) 0.1812(4) 0.0373(14) Uani 0.609(4) 1 d D P A 1
H58A H 0.237040 0.186659 0.192391 0.056 Uiso 0.609(4) 1 calc GR P A 1
H58B H 0.181606 0.096104 0.227102 0.056 Uiso 0.609(4) 1 calc GR P A 1
H58C H 0.120763 0.186988 0.191791 0.056 Uiso 0.609(4) 1 calc GR P A 1
C59 C 0.1231(5) 0.0972(5) 0.0712(4) 0.0438(16) Uani 0.609(4) 1 d D P A 1
H59A H 0.104470 0.148020 0.025160 0.053 Uiso 0.609(4) 1 calc R P A 1
H59B H 0.177278 0.064303 0.057754 0.053 Uiso 0.609(4) 1 calc R P A 1
C62 C 0.1862(8) 0.0992(8) 0.1868(7) 0.047(2) Uani 0.391(4) 1 d D P A 2
H62A H 0.206246 0.046032 0.229600 0.056 Uiso 0.391(4) 1 calc R P A 2
H62B H 0.243100 0.154547 0.211102 0.056 Uiso 0.391(4) 1 calc R P A 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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 0.1284
5 0 -4 0.0541
-1 0 1 0.0584
-1 0 0 0.0845
-4 0 5 0.0761
0 1 0 0.0451
0 -1 0 0.0332
4 1 -5 0.0709
2 -4 5 0.1183
5 3 -2 0.0733
0 4 5 0.1078
5 2 -5 0.0499
19 2 -7 0.0735
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
P3 Pd1 P2 114.88(2) . .
P1 Pd1 P3 126.09(2) . .
P1 Pd1 P2 117.11(2) . .
C37 P3 Pd1 110.83(7) . .
C37 P3 C49 101.07(10) . .
C49 P3 Pd1 121.81(7) . .
C43 P3 Pd1 116.21(7) . .
C43 P3 C37 103.83(10) . .
C43 P3 C49 100.68(10) . .
C25 P2 Pd1 112.71(7) . .
C25 P2 C19 103.50(10) . .
C31 P2 Pd1 119.36(7) . .
C31 P2 C25 101.22(10) . .
C31 P2 C19 100.64(10) . .
C19 P2 Pd1 117.02(7) . .
C13 P1 Pd1 106.23(7) . .
C13 P1 C1 101.18(10) . .
C1 P1 Pd1 123.25(8) . .
C7 P1 Pd1 119.55(7) . .
C7 P1 C13 101.87(10) . .
C7 P1 C1 101.43(10) . .
C26 C25 P2 117.67(17) . .
C26 C25 C30 118.4(2) . .
C30 C25 P2 123.91(17) . .
C38 C37 P3 118.06(17) . .
C38 C37 C42 118.2(2) . .
C42 C37 P3 123.69(17) . .
C50 C49 P3 117.56(17) . .
C54 C49 P3 123.94(17) . .
C54 C49 C50 118.4(2) . .
C25 C26 H26 119.5 . .
C27 C26 C25 121.0(2) . .
C27 C26 H26 119.5 . .
C32 C31 P2 121.83(17) . .
C32 C31 C36 118.0(2) . .
C36 C31 P2 119.92(17) . .
C20 C19 P2 117.17(17) . .
C24 C19 P2 124.26(17) . .
C24 C19 C20 118.6(2) . .
C18 C13 P1 116.55(17) . .
C14 C13 P1 125.23(17) . .
C14 C13 C18 118.2(2) . .
C2 C1 P1 119.21(17) . .
C2 C1 C6 118.5(2) . .
C6 C1 P1 122.30(17) . .
C37 C38 H38 119.7 . .
C39 C38 C37 120.7(2) . .
C39 C38 H38 119.7 . .
C49 C50 H50 119.7 . .
C51 C50 C49 120.6(2) . .
C51 C50 H50 119.7 . .
C13 C18 H18 119.5 . .
C17 C18 C13 121.1(2) . .
C17 C18 H18 119.5 . .
C31 C32 H32 119.4 . .
C31 C32 C33 121.1(2) . .
C33 C32 H32 119.4 . .
C1 C2 H2 119.7 . .
C1 C2 C3 120.7(2) . .
C3 C2 H2 119.7 . .
C49 C54 H54 119.6 . .
C49 C54 C53 120.7(2) . .
C53 C54 H54 119.6 . .
C25 C30 H30 119.7 . .
C29 C30 C25 120.7(2) . .
C29 C30 H30 119.7 . .
C1 C6 H6 119.6 . .
C5 C6 C1 120.8(2) . .
C5 C6 H6 119.6 . .
C31 C36 H36 119.6 . .
C35 C36 C31 120.7(2) . .
C35 C36 H36 119.6 . .
C43 C48 H48 119.5 . .
C47 C48 H48 119.5 . .
C47 C48 C43 120.9(2) . .
C12 C7 P1 124.48(17) . .
C12 C7 C8 117.8(2) . .
C8 C7 P1 117.59(17) . .
C48 C43 P3 116.33(17) . .
C48 C43 C44 118.6(2) . .
C44 C43 P3 125.01(17) . .
C54 C53 H53 119.9 . .
C52 C53 C54 120.1(2) . .
C52 C53 H53 119.9 . .
C19 C20 H20 119.6 . .
C19 C20 C21 120.7(2) . .
C21 C20 H20 119.6 . .
C13 C14 H14 119.7 . .
C13 C14 C15 120.6(2) . .
C15 C14 H14 119.7 . .
C53 C52 H52 120.1 . .
C51 C52 C53 119.8(2) . .
C51 C52 H52 120.1 . .
C43 C44 H44 119.8 . .
C45 C44 C43 120.5(2) . .
C45 C44 H44 119.8 . .
C6 C5 H5 119.9 . .
C6 C5 C4 120.3(2) . .
C4 C5 H5 119.9 . .
C7 C12 H12 119.7 . .
C11 C12 C7 120.6(2) . .
C11 C12 H12 119.7 . .
C8 C9 H9 119.9 . .
C8 C9 C10 120.3(2) . .
C10 C9 H9 119.9 . .
C2 C3 H3 119.9 . .
C4 C3 C2 120.2(2) . .
C4 C3 H3 119.9 . .
C50 C51 H51 119.9 . .
C52 C51 C50 120.3(2) . .
C52 C51 H51 119.9 . .
C36 C35 H35 119.8 . .
C36 C35 C34 120.4(2) . .
C34 C35 H35 119.8 . .
C30 C29 H29 120.0 . .
C30 C29 C28 120.0(2) . .
C28 C29 H29 120.0 . .
C26 C27 H27 120.0 . .
C28 C27 C26 119.9(2) . .
C28 C27 H27 120.0 . .
C35 C34 H34 120.2 . .
C33 C34 C35 119.6(2) . .
C33 C34 H34 120.2 . .
C19 C24 H24 119.7 . .
C23 C24 C19 120.7(2) . .
C23 C24 H24 119.7 . .
C18 C17 H17 119.9 . .
C16 C17 C18 120.3(2) . .
C16 C17 H17 119.9 . .
C7 C8 H8 119.4 . .
C9 C8 C7 121.2(2) . .
C9 C8 H8 119.4 . .
C37 C42 H42 119.6 . .
C41 C42 C37 120.7(2) . .
C41 C42 H42 119.6 . .
C20 C21 H21 120.0 . .
C22 C21 C20 120.0(2) . .
C22 C21 H21 120.0 . .
C44 C45 H45 120.0 . .
C46 C45 C44 120.1(2) . .
C46 C45 H45 120.0 . .
C9 C10 H10 120.4 . .
C11 C10 C9 119.2(2) . .
C11 C10 H10 120.4 . .
C39 C40 H40 120.1 . .
C41 C40 H40 120.1 . .
C41 C40 C39 119.8(2) . .
C5 C4 H4 120.3 . .
C3 C4 C5 119.5(2) . .
C3 C4 H4 120.3 . .
C21 C22 H22 120.0 . .
C21 C22 C23 119.9(2) . .
C23 C22 H22 120.0 . .
C38 C39 H39 119.8 . .
C40 C39 C38 120.3(2) . .
C40 C39 H39 119.8 . .
C42 C41 H41 119.9 . .
C40 C41 C42 120.3(2) . .
C40 C41 H41 119.9 . .
C32 C33 H33 119.9 . .
C34 C33 C32 120.2(2) . .
C34 C33 H33 119.9 . .
C12 C11 H11 119.6 . .
C10 C11 C12 120.8(2) . .
C10 C11 H11 119.6 . .
C29 C28 H28 120.0 . .
C27 C28 C29 120.0(2) . .
C27 C28 H28 120.0 . .
C48 C47 H47 120.0 . .
C46 C47 C48 119.9(2) . .
C46 C47 H47 120.0 . .
C14 C15 H15 119.7 . .
C16 C15 C14 120.6(2) . .
C16 C15 H15 119.7 . .
C24 C23 H23 119.9 . .
C22 C23 C24 120.1(2) . .
C22 C23 H23 119.9 . .
C45 C46 H46 120.0 . .
C47 C46 C45 119.9(2) . .
C47 C46 H46 120.0 . .
C17 C16 C15 119.3(2) . .
C17 C16 H16 120.4 . .
C15 C16 H16 120.4 . .
C57 C57 H57A 108.8 2_676 .
C57 C57 H57B 108.8 2_676 .
H57A C57 H57B 107.7 . .
C56 C57 C57 113.8(3) . 2_676
C56 C57 H57A 108.8 . .
C56 C57 H57B 108.8 . .
C57 C56 H56A 108.8 . .
C57 C56 H56B 108.8 . .
C57 C56 C55 113.8(2) . .
H56A C56 H56B 107.7 . .
C55 C56 H56A 108.8 . .
C55 C56 H56B 108.8 . .
C56 C55 H55A 109.5 . .
C56 C55 H55B 109.5 . .
C56 C55 H55C 109.5 . .
H55A C55 H55B 109.5 . .
H55A C55 H55C 109.5 . .
H55B C55 H55C 109.5 . .
H63A C63 H63B 109.5 . .
C64 C63 H63A 111.8 . .
C64 C63 H63B 111.8 . .
C64 C63 C62 99.8(6) . .
C62 C63 H63A 111.8 . .
C62 C63 H63B 111.8 . .
C64 O1 C61 108.0(6) . .
C60 C60 H60A 108.6 2 .
C60 C60 H60B 108.6 2 .
H60A C60 H60B 107.6 . .
C59 C60 C60 114.5(5) . 2
C59 C60 H60A 108.6 . .
C59 C60 H60B 108.6 . .
C63 C64 H64A 110.4 . .
C63 C64 H64B 110.4 . .
O1 C64 C63 106.4(6) . .
O1 C64 H64A 110.4 . .
O1 C64 H64B 110.4 . .
H64A C64 H64B 108.6 . .
O1 C61 H61A 110.2 . .
O1 C61 H61B 110.2 . .
O1 C61 C62 107.5(6) . .
H61A C61 H61B 108.5 . .
C62 C61 H61A 110.2 . .
C62 C61 H61B 110.2 . .
H58A C58 H58B 109.5 . .
H58A C58 H58C 109.5 . .
H58B C58 H58C 109.5 . .
C59 C58 H58A 109.5 . .
C59 C58 H58B 109.5 . .
C59 C58 H58C 109.5 . .
C60 C59 C58 111.9(4) . .
C60 C59 H59A 109.2 . .
C60 C59 H59B 109.2 . .
C58 C59 H59A 109.2 . .
C58 C59 H59B 109.2 . .
H59A C59 H59B 107.9 . .
C63 C62 H62A 110.5 . .
C63 C62 H62B 110.5 . .
C61 C62 C63 106.0(7) . .
C61 C62 H62A 110.5 . .
C61 C62 H62B 110.5 . .
H62A C62 H62B 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 P3 2.3119(6) .
Pd1 P2 2.3156(6) .
Pd1 P1 2.3084(6) .
P3 C37 1.836(2) .
P3 C49 1.846(2) .
P3 C43 1.831(2) .
P2 C25 1.839(2) .
P2 C31 1.834(2) .
P2 C19 1.841(2) .
P1 C13 1.843(2) .
P1 C1 1.844(2) .
P1 C7 1.843(2) .
C25 C26 1.389(3) .
C25 C30 1.397(3) .
C37 C38 1.396(3) .
C37 C42 1.398(3) .
C49 C50 1.398(3) .
C49 C54 1.391(3) .
C26 H26 0.9300 .
C26 C27 1.387(3) .
C31 C32 1.388(3) .
C31 C36 1.401(3) .
C19 C20 1.389(3) .
C19 C24 1.388(3) .
C13 C18 1.396(3) .
C13 C14 1.387(3) .
C1 C2 1.386(3) .
C1 C6 1.395(3) .
C38 H38 0.9300 .
C38 C39 1.386(3) .
C50 H50 0.9300 .
C50 C51 1.389(3) .
C18 H18 0.9300 .
C18 C17 1.381(3) .
C32 H32 0.9300 .
C32 C33 1.389(3) .
C2 H2 0.9300 .
C2 C3 1.390(3) .
C54 H54 0.9300 .
C54 C53 1.392(3) .
C30 H30 0.9300 .
C30 C29 1.384(3) .
C6 H6 0.9300 .
C6 C5 1.380(3) .
C36 H36 0.9300 .
C36 C35 1.383(3) .
C48 H48 0.9300 .
C48 C43 1.391(3) .
C48 C47 1.387(3) .
C7 C12 1.392(3) .
C7 C8 1.396(3) .
C43 C44 1.392(3) .
C53 H53 0.9300 .
C53 C52 1.383(3) .
C20 H20 0.9300 .
C20 C21 1.392(3) .
C14 H14 0.9300 .
C14 C15 1.388(3) .
C52 H52 0.9300 .
C52 C51 1.380(3) .
C44 H44 0.9300 .
C44 C45 1.390(3) .
C5 H5 0.9300 .
C5 C4 1.386(3) .
C12 H12 0.9300 .
C12 C11 1.387(3) .
C9 H9 0.9300 .
C9 C8 1.381(3) .
C9 C10 1.382(3) .
C3 H3 0.9300 .
C3 C4 1.382(3) .
C51 H51 0.9300 .
C35 H35 0.9300 .
C35 C34 1.384(3) .
C29 H29 0.9300 .
C29 C28 1.386(3) .
C27 H27 0.9300 .
C27 C28 1.381(3) .
C34 H34 0.9300 .
C34 C33 1.378(3) .
C24 H24 0.9300 .
C24 C23 1.386(3) .
C17 H17 0.9300 .
C17 C16 1.380(3) .
C8 H8 0.9300 .
C42 H42 0.9300 .
C42 C41 1.386(3) .
C21 H21 0.9300 .
C21 C22 1.373(3) .
C45 H45 0.9300 .
C45 C46 1.385(4) .
C10 H10 0.9300 .
C10 C11 1.378(4) .
C40 H40 0.9300 .
C40 C39 1.382(4) .
C40 C41 1.380(3) .
C4 H4 0.9300 .
C22 H22 0.9300 .
C22 C23 1.383(3) .
C39 H39 0.9300 .
C41 H41 0.9300 .
C33 H33 0.9300 .
C11 H11 0.9300 .
C28 H28 0.9300 .
C47 H47 0.9300 .
C47 C46 1.381(4) .
C15 H15 0.9300 .
C15 C16 1.383(4) .
C23 H23 0.9300 .
C46 H46 0.9300 .
C16 H16 0.9300 .
C57 C57 1.510(5) 2_676
C57 H57A 0.9700 .
C57 H57B 0.9700 .
C57 C56 1.508(4) .
C56 H56A 0.9700 .
C56 H56B 0.9700 .
C56 C55 1.526(4) .
C55 H55A 0.9600 .
C55 H55B 0.9600 .
C55 H55C 0.9600 .
C63 H63A 0.9700 .
C63 H63B 0.9700 .
C63 C64 1.518(10) .
C63 C62 1.530(11) .
O1 C64 1.404(8) .
O1 C61 1.427(8) .
C60 C60 1.513(8) 2
C60 H60A 0.9700 .
C60 H60B 0.9700 .
C60 C59 1.496(7) .
C64 H64A 0.9700 .
C64 H64B 0.9700 .
C61 H61A 0.9700 .
C61 H61B 0.9700 .
C61 C62 1.479(10) .
C58 H58A 0.9600 .
C58 H58B 0.9600 .
C58 H58C 0.9600 .
C58 C59 1.562(7) .
C59 H59A 0.9700 .
C59 H59B 0.9700 .
C62 H62A 0.9700 .
C62 H62B 0.9700 .
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
Pd1 P3 C37 C38 -23.4(2) .
Pd1 P3 C37 C42 153.85(18) .
Pd1 P3 C49 C50 -50.29(19) .
Pd1 P3 C49 C54 126.74(16) .
Pd1 P3 C43 C48 -33.29(18) .
Pd1 P3 C43 C44 149.20(16) .
Pd1 P2 C25 C26 -21.8(2) .
Pd1 P2 C25 C30 157.04(17) .
Pd1 P2 C31 C32 104.27(17) .
Pd1 P2 C31 C36 -69.88(18) .
Pd1 P2 C19 C20 -27.2(2) .
Pd1 P2 C19 C24 154.25(19) .
Pd1 P1 C13 C18 -37.42(18) .
Pd1 P1 C13 C14 140.28(19) .
Pd1 P1 C1 C2 -18.0(2) .
Pd1 P1 C1 C6 160.81(15) .
Pd1 P1 C7 C12 126.93(18) .
Pd1 P1 C7 C8 -49.4(2) .
P3 C37 C38 C39 175.63(18) .
P3 C37 C42 C41 -175.92(18) .
P3 C49 C50 C51 178.25(17) .
P3 C49 C54 C53 -178.11(16) .
P3 C43 C44 C45 176.93(17) .
P2 C25 C26 C27 179.76(18) .
P2 C25 C30 C29 -179.56(18) .
P2 C31 C32 C33 -174.78(17) .
P2 C31 C36 C35 175.90(17) .
P2 C19 C20 C21 -177.99(19) .
P2 C19 C24 C23 178.6(2) .
P1 C13 C18 C17 177.47(17) .
P1 C13 C14 C15 -178.13(19) .
P1 C1 C2 C3 179.09(18) .
P1 C1 C6 C5 -179.38(18) .
P1 C7 C12 C11 -177.23(19) .
P1 C7 C8 C9 177.73(19) .
C25 P2 C31 C32 -131.46(18) .
C25 P2 C31 C36 54.39(19) .
C25 P2 C19 C20 -151.80(19) .
C25 P2 C19 C24 29.6(2) .
C25 C26 C27 C28 -0.3(4) .
C25 C30 C29 C28 0.0(4) .
C37 P3 C49 C50 72.93(18) .
C37 P3 C49 C54 -110.05(19) .
C37 P3 C43 C48 -155.26(16) .
C37 P3 C43 C44 27.2(2) .
C37 C38 C39 C40 0.7(4) .
C37 C42 C41 C40 0.2(4) .
C49 P3 C37 C38 -153.84(18) .
C49 P3 C37 C42 23.4(2) .
C49 P3 C43 C48 100.40(17) .
C49 P3 C43 C44 -77.1(2) .
C49 C50 C51 C52 -0.5(3) .
C49 C54 C53 C52 0.6(3) .
C26 C25 C30 C29 -0.8(3) .
C26 C27 C28 C29 -0.5(4) .
C31 P2 C25 C26 -150.43(18) .
C31 P2 C25 C30 28.4(2) .
C31 P2 C19 C20 103.80(19) .
C31 P2 C19 C24 -74.8(2) .
C31 C32 C33 C34 -0.6(3) .
C31 C36 C35 C34 -1.4(3) .
C19 P2 C25 C26 105.61(18) .
C19 P2 C25 C30 -75.6(2) .
C19 P2 C31 C32 -25.2(2) .
C19 P2 C31 C36 160.62(17) .
C19 C20 C21 C22 -0.8(4) .
C19 C24 C23 C22 -0.7(4) .
C13 P1 C1 C2 -136.04(18) .
C13 P1 C1 C6 42.8(2) .
C13 P1 C7 C12 -116.5(2) .
C13 P1 C7 C8 67.23(19) .
C13 C18 C17 C16 0.9(4) .
C13 C14 C15 C16 0.8(4) .
C1 P1 C13 C18 92.35(18) .
C1 P1 C13 C14 -90.0(2) .
C1 P1 C7 C12 -12.3(2) .
C1 P1 C7 C8 171.39(18) .
C1 C2 C3 C4 0.1(4) .
C1 C6 C5 C4 0.5(4) .
C38 C37 C42 C41 1.3(3) .
C50 C49 C54 C53 -1.1(3) .
C18 C13 C14 C15 -0.5(4) .
C18 C17 C16 C15 -0.6(4) .
C32 C31 C36 C35 1.5(3) .
C2 C1 C6 C5 -0.6(3) .
C2 C3 C4 C5 -0.2(4) .
C54 C49 C50 C51 1.1(3) .
C54 C53 C52 C51 0.0(3) .
C30 C25 C26 C27 0.9(3) .
C30 C29 C28 C27 0.6(4) .
C6 C1 C2 C3 0.3(3) .
C6 C5 C4 C3 -0.1(4) .
C36 C31 C32 C33 -0.5(3) .
C36 C35 C34 C33 0.2(3) .
C48 C43 C44 C45 -0.5(3) .
C48 C47 C46 C45 -0.3(3) .
C7 P1 C13 C18 -163.29(17) .
C7 P1 C13 C14 14.4(2) .
C7 P1 C1 C2 119.25(18) .
C7 P1 C1 C6 -61.9(2) .
C7 C12 C11 C10 0.1(4) .
C43 P3 C37 C38 102.12(19) .
C43 P3 C37 C42 -80.7(2) .
C43 P3 C49 C50 179.48(17) .
C43 P3 C49 C54 -3.5(2) .
C43 C48 C47 C46 -1.1(3) .
C43 C44 C45 C46 -0.9(3) .
C53 C52 C51 C50 0.0(3) .
C20 C19 C24 C23 0.1(4) .
C20 C21 C22 C23 0.3(4) .
C14 C13 C18 C17 -0.4(3) .
C14 C15 C16 C17 -0.3(4) .
C44 C45 C46 C47 1.3(3) .
C12 C7 C8 C9 1.2(4) .
C9 C10 C11 C12 0.5(4) .
C35 C34 C33 C32 0.8(3) .
C24 C19 C20 C21 0.7(4) .
C8 C7 C12 C11 -1.0(4) .
C8 C9 C10 C11 -0.3(4) .
C42 C37 C38 C39 -1.7(3) .
C21 C22 C23 C24 0.5(4) .
C10 C9 C8 C7 -0.6(4) .
C39 C40 C41 C42 -1.2(4) .
C41 C40 C39 C38 0.8(4) .
C47 C48 C43 P3 -176.12(17) .
C47 C48 C43 C44 1.6(3) .
C57 C57 C56 C55 -177.1(3) 2_676
O1 C61 C62 C63 -8.7(11) .
C60 C60 C59 C58 177.8(6) 2
C64 C63 C62 C61 25.8(11) .
C64 O1 C61 C62 -14.1(9) .
C61 O1 C64 C63 31.7(9) .
C62 C63 C64 O1 -35.0(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 0.0000 1.0000 0.0009 0.0411 0.0338
5.0000 0.0000 -4.0000 0.0324 0.0817 -0.2719
-1.0000 -0.0000 1.0000 -0.0063 -0.0081 0.0611
-1.0000 -0.0000 0.0000 -0.0072 -0.0492 0.0274
-4.0000 -0.0000 5.0000 -0.0242 0.0087 0.2783
-0.0000 1.0000 0.0000 -0.0506 0.0123 -0.0061
0.0000 -1.0000 -0.0000 0.0506 -0.0123 0.0061
4.0000 1.0000 -5.0000 -0.0264 0.0036 -0.2844
2.0000 -4.0000 5.0000 0.2216 0.2551 0.1383
5.0000 3.0000 -2.0000 -0.1175 0.2007 -0.2226
-0.0000 4.0000 5.0000 -0.1976 0.2546 0.1445
5.0000 2.0000 -5.0000 -0.0697 0.0651 -0.3178
19.0000 2.0000 -7.0000 0.0298 0.6722 -0.7685
