#------------------------------------------------------------------------------
#$Date: 2020-03-04 03:41:19 +0200 (Wed, 04 Mar 2020) $
#$Revision: 248712 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/41/4134143.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_4134143
loop_
_publ_author_name
'de Gombert, Antoine'
'McKay, Alasdair I.'
'Davis, Christopher J.'
'Wheelhouse, Katherine M.'
'Willis, Michael C.'
_publ_section_title
;
 Mechanistic Studies of the Palladium-Catalyzed Desulfinative
 Cross-Coupling of Aryl Bromides and (Hetero)Aryl Sulfinate Salts.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3564
_journal_page_last               3576
_journal_paper_doi               10.1021/jacs.9b13260
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C29 H41 F N O2 P Pd S, C3 H7'
_chemical_formula_sum            'C32 H48 F N O2 P Pd S'
_chemical_formula_weight         667.14
_chemical_name_common            (4-F-C6H4)Pd(PCy3)(SO2C6H4N)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 130.842(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.707(2)
_cell_length_b                   9.0995(3)
_cell_length_c                   27.7743(18)
_cell_measurement_reflns_used    14888
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      29.2210
_cell_measurement_theta_min      1.9280
_cell_volume                     6444.6(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.12b (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      169.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -74.00 110.00   0.50   14.93    --   20.00  54.00 -39.69  368
  2  ω    -74.00 110.00   0.50   14.93    --   20.00  54.00-138.43  368
  3  ω    -74.00 110.00   0.50   14.93    --   20.00  54.00  89.68  368
  4  ω    -74.00 110.00   0.50   14.93    --   20.00  54.00-102.76  368
  5  ω    -74.00 110.00   0.50   14.93    --   20.00  54.00-180.00  368
  6  ω    -74.00 110.00   0.50   14.93    --   20.00  54.00-180.00  368
  7  ω    -22.00  90.00   0.50   14.93    --   20.00  54.00  60.00  224
  8  ω    -74.00  90.00   0.50   14.93    --   20.00  54.00 -77.28  328
  9  ω    -69.00  40.00   0.50   14.93    --   20.00  54.00   0.00  218
 10  ω    -73.00  97.00   0.50   14.93    --   20.00  54.00 120.00  340
 11  ω    -73.00 -26.00   0.50   14.93    --   20.00  54.00-116.79   94
 12  ω    -18.00   8.00   0.50   14.93    --   20.00  54.00-116.79   52
 13  ω    -62.00 -10.00   0.50   14.93    --   20.00  54.00 -30.00  104
 14  ω    -74.00  66.00   0.50   14.93    --   20.00  54.00-171.23  280
 15  ω    -64.00 -30.00   0.50   14.93    --   20.00  54.00  73.58   68
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0061243000
_diffrn_orient_matrix_UB_12      0.0175101000
_diffrn_orient_matrix_UB_13      0.0290957000
_diffrn_orient_matrix_UB_21      0.0251904000
_diffrn_orient_matrix_UB_22      0.0244523000
_diffrn_orient_matrix_UB_23      0.0127224000
_diffrn_orient_matrix_UB_31      -0.0100611000
_diffrn_orient_matrix_UB_32      0.0719783000
_diffrn_orient_matrix_UB_33      -0.0113559000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            92978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.938
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.12b (Rigaku Oxford Diffraction, 2018)
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    1.375
_exptl_crystal_description       plank
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7123
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0354P)²+10.9273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5559
_reflns_number_total             7123
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b13260_si_001.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 4134138--4134148.cif.'
_cod_original_cell_volume        6444.7(10)
_cod_database_code               4134143
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pd N F P S O2  C28 H41'
_chemical_oxdiff_usercomment     'NMR tube crystals'
_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   0.993
_shelx_estimated_absorpt_t_min   0.670
_reflns_odcompleteness_completeness 99.94
_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,H,H,H) groups
2. Restrained distances
 C32-C31 = C31A-C32A = C31A-C30 = C31-C30
 1.5 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C30 \\sim C31A \\sim C32: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 C30, C31, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C31A, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=
 Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C31)=Sof(H31C)=
 Sof(H31D)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C1(H1), C13(H13)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C2(H2A,H2B), C6(H6A,H6B), C12(H12A,H12B), C8(H8A,H8B), C5(H5A,
 H5B), C4(H4A,H4B), C3(H3A,H3B), C18(H18A,H18B), C15(H15A,H15B), C17(H17A,H17B),
  C11(H11A,H11B), C9(H9A,H9B), C16(H16A,H16B), C10(H10A,H10B), C32(H32A,H32B),
 C31A(H31A,H31B), C31(H31C,H31D), C32A(H32C,H32D)
6.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C20(H20), C24(H24), C27(H27), C23(H23), C21(H21), C25(H25), C26(H26)
6.d Idealised Me refined as rotating group:
 C30(H30D,H30E,H30F), C30(H30A,H30B,H30C)
;
_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 1.362
_oxdiff_exptl_absorpt_empirical_full_min 0.735
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.62619(2) 0.44928(2) 0.70981(2) 0.02212(7) Uani 1 1 d . . . . .
P1 P 0.56499(3) 0.26952(8) 0.66041(3) 0.02154(16) Uani 1 1 d . . . . .
S1 S 0.62098(3) 0.66674(9) 0.62155(4) 0.03037(18) Uani 1 1 d . . . . .
O1 O 0.58487(8) 0.5923(2) 0.62950(10) 0.0291(5) Uani 1 1 d . . . . .
F1 F 0.77260(8) 0.1353(3) 0.96722(9) 0.0560(6) Uani 1 1 d . . . . .
O2 O 0.64675(9) 0.5556(3) 0.61065(10) 0.0380(5) Uani 1 1 d . . . . .
N1 N 0.68269(9) 0.6232(3) 0.74847(11) 0.0257(5) Uani 1 1 d . . . . .
C19 C 0.66979(11) 0.3370(3) 0.79048(13) 0.0249(6) Uani 1 1 d . . . . .
C28 C 0.70684(12) 0.8356(3) 0.72166(16) 0.0332(7) Uani 1 1 d . . . . .
H28 H 0.700474 0.897001 0.690485 0.040 Uiso 1 1 calc R . . . .
C14 C 0.49942(12) 0.4404(3) 0.66966(15) 0.0318(7) Uani 1 1 d . . . . .
H14A H 0.502288 0.373240 0.698930 0.038 Uiso 1 1 calc R . . . .
H14B H 0.529006 0.507299 0.694309 0.038 Uiso 1 1 calc R . . . .
C7 C 0.57745(12) 0.1037(3) 0.70779(14) 0.0261(6) Uani 1 1 d . . . . .
H7 H 0.615675 0.092433 0.738091 0.031 Uiso 1 1 calc R . . . .
C2 C 0.61259(11) 0.1509(4) 0.61737(14) 0.0293(7) Uani 1 1 d . . . . .
H2A H 0.635276 0.236357 0.633820 0.035 Uiso 1 1 calc R . . . .
H2B H 0.628098 0.081299 0.651963 0.035 Uiso 1 1 calc R . . . .
C20 C 0.66738(12) 0.3649(4) 0.83802(14) 0.0312(7) Uani 1 1 d . . . . .
H20 H 0.642388 0.430340 0.829804 0.037 Uiso 1 1 calc R . . . .
C29 C 0.67498(11) 0.7148(3) 0.70509(14) 0.0261(6) Uani 1 1 d . . . . .
C6 C 0.53198(12) 0.3031(3) 0.53624(14) 0.0285(7) Uani 1 1 d . . . . .
H6A H 0.497129 0.328265 0.519905 0.034 Uiso 1 1 calc R . . . .
H6B H 0.552301 0.392929 0.550067 0.034 Uiso 1 1 calc R . . . .
C24 C 0.70873(11) 0.2401(3) 0.80553(13) 0.0276(6) Uani 1 1 d . . . . .
H24 H 0.711104 0.219179 0.774715 0.033 Uiso 1 1 calc R . . . .
C1 C 0.55824(11) 0.1975(3) 0.59295(13) 0.0241(6) Uani 1 1 d . . . . .
H1 H 0.536498 0.108836 0.577382 0.029 Uiso 1 1 calc R . . . .
C13 C 0.50076(11) 0.3531(3) 0.62328(13) 0.0252(6) Uani 1 1 d . . . . .
H13 H 0.495245 0.426575 0.593593 0.030 Uiso 1 1 calc R . . . .
C12 C 0.56287(12) 0.1243(3) 0.74951(14) 0.0308(7) Uani 1 1 d . . . . .
H12A H 0.577136 0.216656 0.772365 0.037 Uiso 1 1 calc R . . . .
H12B H 0.525016 0.128442 0.722641 0.037 Uiso 1 1 calc R . . . .
C22 C 0.73881(12) 0.2034(4) 0.90885(14) 0.0369(8) Uani 1 1 d . . . . .
C8 C 0.55643(13) -0.0449(3) 0.67296(15) 0.0335(7) Uani 1 1 d . . . . .
H8A H 0.518435 -0.045438 0.644502 0.040 Uiso 1 1 calc R . . . .
H8B H 0.566547 -0.059037 0.647642 0.040 Uiso 1 1 calc R . . . .
C5 C 0.52826(12) 0.2306(4) 0.48367(14) 0.0333(7) Uani 1 1 d . . . . .
H5A H 0.505853 0.144691 0.467968 0.040 Uiso 1 1 calc R . . . .
H5B H 0.512358 0.298855 0.448545 0.040 Uiso 1 1 calc R . . . .
C27 C 0.74826(13) 0.8628(4) 0.78543(17) 0.0403(8) Uani 1 1 d . . . . .
H27 H 0.770328 0.942656 0.797870 0.048 Uiso 1 1 calc R . . . .
C23 C 0.74396(12) 0.1740(4) 0.86491(14) 0.0328(7) Uani 1 1 d . . . . .
H23 H 0.770191 0.111920 0.874443 0.039 Uiso 1 1 calc R . . . .
C4 C 0.58214(13) 0.1848(4) 0.50765(15) 0.0384(8) Uani 1 1 d . . . . .
H4A H 0.603769 0.271407 0.520227 0.046 Uiso 1 1 calc R . . . .
H4B H 0.578279 0.136351 0.473688 0.046 Uiso 1 1 calc R . . . .
C21 C 0.70149(13) 0.2971(4) 0.89744(15) 0.0383(8) Uani 1 1 d . . . . .
H21 H 0.699064 0.314775 0.928412 0.046 Uiso 1 1 calc R . . . .
C3 C 0.60886(14) 0.0807(4) 0.56443(15) 0.0362(8) Uani 1 1 d . . . . .
H3A H 0.643783 0.057098 0.580655 0.043 Uiso 1 1 calc R . . . .
H3B H 0.589022 -0.010047 0.550764 0.043 Uiso 1 1 calc R . . . .
C18 C 0.45296(11) 0.2488(4) 0.58174(15) 0.0316(7) Uani 1 1 d . . . . .
H18A H 0.453493 0.198011 0.551458 0.038 Uiso 1 1 calc R . . . .
H18B H 0.454679 0.175743 0.608501 0.038 Uiso 1 1 calc R . . . .
C25 C 0.72331(12) 0.6498(4) 0.81065(15) 0.0334(7) Uani 1 1 d . . . . .
H25 H 0.729352 0.586382 0.841104 0.040 Uiso 1 1 calc R . . . .
C26 C 0.75630(13) 0.7697(4) 0.83026(17) 0.0404(8) Uani 1 1 d . . . . .
H26 H 0.783649 0.787047 0.873381 0.048 Uiso 1 1 calc R . . . .
C15 C 0.44822(13) 0.5277(4) 0.63303(18) 0.0413(8) Uani 1 1 d . . . . .
H15A H 0.447220 0.578744 0.662890 0.050 Uiso 1 1 calc R . . . .
H15B H 0.446781 0.600684 0.606461 0.050 Uiso 1 1 calc R . . . .
C17 C 0.40220(12) 0.3375(4) 0.54614(16) 0.0420(8) Uani 1 1 d . . . . .
H17A H 0.399116 0.403843 0.516497 0.050 Uiso 1 1 calc R . . . .
H17B H 0.372460 0.271111 0.521829 0.050 Uiso 1 1 calc R . . . .
C11 C 0.58425(16) -0.0019(4) 0.79712(17) 0.0437(9) Uani 1 1 d . . . . .
H11A H 0.622276 0.000642 0.826819 0.052 Uiso 1 1 calc R . . . .
H11B H 0.572908 0.010847 0.821188 0.052 Uiso 1 1 calc R . . . .
C9 C 0.57844(15) -0.1702(4) 0.72112(17) 0.0425(9) Uani 1 1 d . . . . .
H9A H 0.564011 -0.262760 0.698501 0.051 Uiso 1 1 calc R . . . .
H9B H 0.616210 -0.174242 0.747148 0.051 Uiso 1 1 calc R . . . .
C16 C 0.40099(13) 0.4257(4) 0.59158(18) 0.0463(9) Uani 1 1 d . . . . .
H16A H 0.400717 0.358922 0.618581 0.056 Uiso 1 1 calc R . . . .
H16B H 0.369053 0.483480 0.567347 0.056 Uiso 1 1 calc R . . . .
C10 C 0.56552(17) -0.1507(4) 0.76388(19) 0.0491(10) Uani 1 1 d . . . . .
H10A H 0.582157 -0.228210 0.795545 0.059 Uiso 1 1 calc R . . . .
H10B H 0.527915 -0.158565 0.738594 0.059 Uiso 1 1 calc R . . . .
C30 C 0.6771(3) -0.0355(7) 0.9849(3) 0.106(2) Uani 1 1 d D U . . .
H30D H 0.710969 -0.011262 1.024555 0.160 Uiso 0.47(3) 1 calc GR . P A 2
H30E H 0.651058 -0.023836 0.988978 0.160 Uiso 0.47(3) 1 calc GR . P A 2
H30F H 0.669072 0.028584 0.952114 0.160 Uiso 0.47(3) 1 calc GR . P A 2
H30A H 0.639683 -0.033857 0.959367 0.160 Uiso 0.53(3) 1 calc GR . P A 1
H30B H 0.687308 0.041686 0.971448 0.160 Uiso 0.53(3) 1 calc GR . P A 1
H30C H 0.693783 -0.021245 1.028793 0.160 Uiso 0.53(3) 1 calc GR . P A 1
C32 C 0.7209(9) -0.2514(18) 0.9651(9) 0.095(6) Uani 0.53(3) 1 d D U P A 1
H32A H 0.720283 -0.202727 0.933475 0.113 Uiso 0.53(3) 1 calc R . P A 1
H32B H 0.707800 -0.350910 0.951212 0.113 Uiso 0.53(3) 1 calc R . P A 1
C31A C 0.6772(8) -0.193(3) 0.9678(8) 0.081(4) Uani 0.47(3) 1 d D U P A 2
H31A H 0.654847 -0.208220 0.922238 0.097 Uiso 0.47(3) 1 calc R . P A 2
H31B H 0.668783 -0.262382 0.986335 0.097 Uiso 0.47(3) 1 calc R . P A 2
C31 C 0.6921(12) -0.170(3) 0.9778(15) 0.180(11) Uani 0.53(3) 1 d D U P A 1
H31C H 0.657842 -0.214913 0.946507 0.216 Uiso 0.53(3) 1 calc R . P A 1
H31D H 0.705827 -0.216254 1.017617 0.216 Uiso 0.53(3) 1 calc R . P A 1
C32A C 0.7393(9) -0.189(3) 1.0037(17) 0.134(10) Uani 0.47(3) 1 d D U P A 2
H32C H 0.745656 -0.102751 0.989156 0.160 Uiso 0.47(3) 1 calc R . P A 2
H32D H 0.758760 -0.176538 1.048834 0.160 Uiso 0.47(3) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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
O1 Pd1 P1 95.41(6) . .
O1 Pd1 N1 80.33(9) . .
N1 Pd1 P1 174.65(7) . .
C19 Pd1 P1 91.20(8) . .
C19 Pd1 O1 173.16(10) . .
C19 Pd1 N1 93.17(10) . .
C7 P1 Pd1 117.59(10) . .
C1 P1 Pd1 109.24(10) . .
C1 P1 C7 104.47(13) . .
C13 P1 Pd1 108.18(10) . .
C13 P1 C7 111.66(13) . .
C13 P1 C1 104.91(13) . .
O1 S1 C29 98.51(13) . .
O2 S1 O1 110.74(13) . .
O2 S1 C29 101.00(13) . .
S1 O1 Pd1 112.59(11) . .
C29 N1 Pd1 114.88(19) . .
C29 N1 C25 118.4(3) . .
C25 N1 Pd1 126.7(2) . .
C20 C19 Pd1 121.1(2) . .
C20 C19 C24 117.0(3) . .
C24 C19 Pd1 121.4(2) . .
C29 C28 H28 120.6 . .
C27 C28 H28 120.6 . .
C27 C28 C29 118.7(3) . .
H14A C14 H14B 108.1 . .
C13 C14 H14A 109.6 . .
C13 C14 H14B 109.6 . .
C15 C14 H14A 109.6 . .
C15 C14 H14B 109.6 . .
C15 C14 C13 110.4(3) . .
P1 C7 H7 104.7 . .
C12 C7 P1 113.5(2) . .
C12 C7 H7 104.7 . .
C12 C7 C8 109.8(2) . .
C8 C7 P1 118.0(2) . .
C8 C7 H7 104.7 . .
H2A C2 H2B 108.0 . .
C1 C2 H2A 109.3 . .
C1 C2 H2B 109.3 . .
C3 C2 H2A 109.3 . .
C3 C2 H2B 109.3 . .
C3 C2 C1 111.4(2) . .
C19 C20 H20 119.2 . .
C21 C20 C19 121.7(3) . .
C21 C20 H20 119.2 . .
N1 C29 S1 115.9(2) . .
N1 C29 C28 122.7(3) . .
C28 C29 S1 121.4(2) . .
H6A C6 H6B 108.2 . .
C1 C6 H6A 109.7 . .
C1 C6 H6B 109.7 . .
C5 C6 H6A 109.7 . .
C5 C6 H6B 109.7 . .
C5 C6 C1 109.9(2) . .
C19 C24 H24 118.9 . .
C23 C24 C19 122.3(3) . .
C23 C24 H24 118.9 . .
P1 C1 H1 107.4 . .
C2 C1 P1 109.15(19) . .
C2 C1 H1 107.4 . .
C6 C1 P1 115.0(2) . .
C6 C1 C2 110.2(2) . .
C6 C1 H1 107.4 . .
P1 C13 H13 105.0 . .
C14 C13 P1 114.3(2) . .
C14 C13 H13 105.0 . .
C14 C13 C18 110.7(2) . .
C18 C13 P1 115.6(2) . .
C18 C13 H13 105.0 . .
C7 C12 H12A 109.4 . .
C7 C12 H12B 109.4 . .
H12A C12 H12B 108.0 . .
C11 C12 C7 110.9(3) . .
C11 C12 H12A 109.4 . .
C11 C12 H12B 109.4 . .
C23 C22 F1 118.3(3) . .
C23 C22 C21 123.2(3) . .
C21 C22 F1 118.6(3) . .
C7 C8 H8A 109.6 . .
C7 C8 H8B 109.6 . .
H8A C8 H8B 108.1 . .
C9 C8 C7 110.1(3) . .
C9 C8 H8A 109.6 . .
C9 C8 H8B 109.6 . .
C6 C5 H5A 109.3 . .
C6 C5 H5B 109.3 . .
H5A C5 H5B 107.9 . .
C4 C5 C6 111.7(3) . .
C4 C5 H5A 109.3 . .
C4 C5 H5B 109.3 . .
C28 C27 H27 120.5 . .
C26 C27 C28 119.0(3) . .
C26 C27 H27 120.5 . .
C24 C23 H23 121.1 . .
C22 C23 C24 117.8(3) . .
C22 C23 H23 121.1 . .
C5 C4 H4A 109.6 . .
C5 C4 H4B 109.6 . .
C5 C4 C3 110.4(3) . .
H4A C4 H4B 108.1 . .
C3 C4 H4A 109.6 . .
C3 C4 H4B 109.6 . .
C20 C21 H21 121.0 . .
C22 C21 C20 118.0(3) . .
C22 C21 H21 121.0 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
C4 C3 C2 110.8(3) . .
C4 C3 H3A 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 108.1 . .
C13 C18 H18A 109.7 . .
C13 C18 H18B 109.7 . .
H18A C18 H18B 108.2 . .
C17 C18 C13 109.7(3) . .
C17 C18 H18A 109.7 . .
C17 C18 H18B 109.7 . .
N1 C25 H25 119.2 . .
N1 C25 C26 121.6(3) . .
C26 C25 H25 119.2 . .
C27 C26 C25 119.6(3) . .
C27 C26 H26 120.2 . .
C25 C26 H26 120.2 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 108.1 . .
C16 C15 C14 110.6(3) . .
C16 C15 H15A 109.5 . .
C16 C15 H15B 109.5 . .
C18 C17 H17A 109.3 . .
C18 C17 H17B 109.3 . .
H17A C17 H17B 108.0 . .
C16 C17 C18 111.6(3) . .
C16 C17 H17A 109.3 . .
C16 C17 H17B 109.3 . .
C12 C11 H11A 109.3 . .
C12 C11 H11B 109.3 . .
H11A C11 H11B 108.0 . .
C10 C11 C12 111.7(3) . .
C10 C11 H11A 109.3 . .
C10 C11 H11B 109.3 . .
C8 C9 H9A 109.2 . .
C8 C9 H9B 109.2 . .
H9A C9 H9B 107.9 . .
C10 C9 C8 111.9(3) . .
C10 C9 H9A 109.2 . .
C10 C9 H9B 109.2 . .
C15 C16 H16A 109.3 . .
C15 C16 H16B 109.3 . .
C17 C16 C15 111.5(3) . .
C17 C16 H16A 109.3 . .
C17 C16 H16B 109.3 . .
H16A C16 H16B 108.0 . .
C11 C10 H10A 109.4 . .
C11 C10 H10B 109.4 . .
C9 C10 C11 111.2(3) . .
C9 C10 H10A 109.4 . .
C9 C10 H10B 109.4 . .
H10A C10 H10B 108.0 . .
H30D C30 H30E 109.5 . .
H30D C30 H30F 109.5 . .
H30E C30 H30F 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C31A C30 H30D 109.5 . .
C31A C30 H30E 109.5 . .
C31A C30 H30F 109.5 . .
C31 C30 H30A 109.5 . .
C31 C30 H30B 109.5 . .
C31 C30 H30C 109.5 . .
C32 C32 H32A 111.7 7_647 .
C32 C32 H32B 111.7 7_647 .
H32A C32 H32B 109.5 . .
C31 C32 C32 100.3(19) . 7_647
C31 C32 H32A 111.7 . .
C31 C32 H32B 111.7 . .
C30 C31A H31A 113.1 . .
C30 C31A H31B 113.1 . .
C30 C31A C32A 93.3(18) . .
H31A C31A H31B 110.4 . .
C32A C31A H31A 113.1 . .
C32A C31A H31B 113.1 . .
C30 C31 C32 149(3) . .
C30 C31 H31C 99.5 . .
C30 C31 H31D 99.5 . .
C32 C31 H31C 99.5 . .
C32 C31 H31D 99.5 . .
H31C C31 H31D 104.1 . .
C31A C32A H32C 107.8 . .
C31A C32A H32D 107.8 . .
C32A C32A C31A 118(4) 7_647 .
C32A C32A H32C 107.8 7_647 .
C32A C32A H32D 107.8 7_647 .
H32C C32A H32D 107.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 P1 2.2608(8) .
Pd1 O1 2.132(2) .
Pd1 N1 2.147(2) .
Pd1 C19 1.979(3) .
P1 C7 1.861(3) .
P1 C1 1.853(3) .
P1 C13 1.846(3) .
S1 O1 1.530(2) .
S1 O2 1.488(2) .
S1 C29 1.834(3) .
F1 C22 1.376(3) .
N1 C29 1.343(4) .
N1 C25 1.350(4) .
C19 C20 1.398(4) .
C19 C24 1.399(4) .
C28 H28 0.9300 .
C28 C29 1.388(4) .
C28 C27 1.383(5) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C14 C13 1.539(4) .
C14 C15 1.532(4) .
C7 H7 0.9800 .
C7 C12 1.538(4) .
C7 C8 1.540(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 C1 1.540(4) .
C2 C3 1.531(4) .
C20 H20 0.9300 .
C20 C21 1.394(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C1 1.538(4) .
C6 C5 1.531(4) .
C24 H24 0.9300 .
C24 C23 1.389(4) .
C1 H1 0.9800 .
C13 H13 0.9800 .
C13 C18 1.548(4) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 C11 1.530(4) .
C22 C23 1.367(4) .
C22 C21 1.374(5) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 C9 1.530(4) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 C4 1.528(4) .
C27 H27 0.9300 .
C27 C26 1.378(5) .
C23 H23 0.9300 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C3 1.529(4) .
C21 H21 0.9300 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C18 C17 1.531(4) .
C25 H25 0.9300 .
C25 C26 1.390(4) .
C26 H26 0.9300 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C15 C16 1.525(5) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 C16 1.518(5) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C11 C10 1.523(5) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 C10 1.519(5) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C30 H30D 0.9600 .
C30 H30E 0.9600 .
C30 H30F 0.9600 .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C30 C31A 1.51(2) .
C30 C31 1.39(3) .
C32 C32 1.62(4) 7_647
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C32 C31 1.44(3) .
C31A H31A 0.9700 .
C31A H31B 0.9700 .
C31A C32A 1.63(3) .
C31 H31C 0.9700 .
C31 H31D 0.9700 .
C32A C32A 1.40(6) 7_647
C32A H32C 0.9700 .
C32A H32D 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
_geom_torsion_site_symmetry_4
Pd1 P1 C7 C12 81.8(2) . .
Pd1 P1 C7 C8 -147.7(2) . .
Pd1 P1 C1 C2 53.8(2) . .
Pd1 P1 C1 C6 -70.6(2) . .
Pd1 P1 C13 C14 -55.2(2) . .
Pd1 P1 C13 C18 174.56(19) . .
Pd1 N1 C29 S1 -4.2(3) . .
Pd1 N1 C29 C28 178.2(2) . .
Pd1 N1 C25 C26 -177.4(2) . .
Pd1 C19 C20 C21 -173.6(2) . .
Pd1 C19 C24 C23 171.9(2) . .
P1 C7 C12 C11 -168.2(2) . .
P1 C7 C8 C9 170.3(2) . .
P1 C13 C18 C17 -171.3(2) . .
O1 S1 C29 N1 30.9(2) . .
O1 S1 C29 C28 -151.5(2) . .
F1 C22 C23 C24 178.2(3) . .
F1 C22 C21 C20 -179.8(3) . .
O2 S1 O1 Pd1 61.88(15) . .
O2 S1 C29 N1 -82.3(2) . .
O2 S1 C29 C28 95.3(3) . .
N1 C25 C26 C27 -1.2(5) . .
C19 C20 C21 C22 1.4(5) . .
C19 C24 C23 C22 1.7(5) . .
C28 C27 C26 C25 0.9(5) . .
C14 C13 C18 C17 56.7(3) . .
C14 C15 C16 C17 -56.4(4) . .
C7 P1 C1 C2 -72.8(2) . .
C7 P1 C1 C6 162.8(2) . .
C7 P1 C13 C14 75.8(2) . .
C7 P1 C13 C18 -54.5(3) . .
C7 C12 C11 C10 -55.9(4) . .
C7 C8 C9 C10 57.1(4) . .
C20 C19 C24 C23 -0.3(4) . .
C29 S1 O1 Pd1 -43.38(14) . .
C29 N1 C25 C26 0.9(5) . .
C29 C28 C27 C26 -0.3(5) . .
C6 C5 C4 C3 57.3(4) . .
C24 C19 C20 C21 -1.3(5) . .
C1 P1 C7 C12 -156.9(2) . .
C1 P1 C7 C8 -26.5(3) . .
C1 P1 C13 C14 -171.7(2) . .
C1 P1 C13 C18 58.0(2) . .
C1 C2 C3 C4 56.3(4) . .
C1 C6 C5 C4 -57.7(3) . .
C13 P1 C7 C12 -44.1(3) . .
C13 P1 C7 C8 86.4(2) . .
C13 P1 C1 C2 169.6(2) . .
C13 P1 C1 C6 45.2(2) . .
C13 C14 C15 C16 56.7(4) . .
C13 C18 C17 C16 -56.2(4) . .
C12 C7 C8 C9 -57.6(3) . .
C12 C11 C10 C9 54.2(4) . .
C8 C7 C12 C11 57.3(3) . .
C8 C9 C10 C11 -55.1(4) . .
C5 C6 C1 P1 -179.5(2) . .
C5 C6 C1 C2 56.7(3) . .
C5 C4 C3 C2 -55.9(4) . .
C27 C28 C29 S1 -177.4(2) . .
C27 C28 C29 N1 0.0(5) . .
C23 C22 C21 C20 0.1(5) . .
C21 C22 C23 C24 -1.6(5) . .
C3 C2 C1 P1 176.1(2) . .
C3 C2 C1 C6 -56.7(3) . .
C18 C17 C16 C15 56.7(4) . .
C25 N1 C29 S1 177.3(2) . .
C25 N1 C29 C28 -0.3(4) . .
C15 C14 C13 P1 169.9(2) . .
C15 C14 C13 C18 -57.5(3) . .
C30 C31A C32A C32A -173(3) . 7_647
C32 C32 C31 C30 82(6) 7_647 .
