# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CVC613_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc1plpnm
_database_code_depnum_ccdc_archive 'CCDC 1567101'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/acscatal.7b02356 2017
_audit_update_record             
;
2017-08-06 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 O4 Pd S2'
_chemical_formula_weight         496.89

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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0235(3)
_cell_length_b                   10.1775(4)
_cell_length_c                   11.8976(5)
_cell_angle_alpha                81.443(2)
_cell_angle_beta                 73.982(2)
_cell_angle_gamma                76.298(2)
_cell_volume                     1016.25(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    126
_cell_measurement_theta_min      4.0035
_cell_measurement_theta_max      27.9018

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_F_000             504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.479
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.114
_exptl_absorpt_coefficient_mu    1.141
_shelx_estimated_absorpt_T_min   0.611
_shelx_estimated_absorpt_T_max   0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO PHOTON 50'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15108
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.609
_diffrn_reflns_theta_max         25.035
_diffrn_reflns_theta_full        25.035
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3577
_reflns_number_gt                3128
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+0.2968P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3577
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.1067
_refine_ls_wR_factor_gt          0.0915
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_restrained_S_all      0.883
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.29686(3) 0.55599(2) 0.30546(2) 0.01776(13) Uani 1 1 d . . . . .
S1 S 0.42914(9) 0.39888(8) 0.41697(7) 0.0186(2) Uani 1 1 d . . . . .
S2 S 0.43562(10) 0.71951(8) 0.28728(7) 0.0187(2) Uani 1 1 d . . . . .
O1 O 0.1637(2) 0.4182(2) 0.31668(19) 0.0171(5) Uani 1 1 d . . . . .
O2 O 0.1734(3) 0.6870(2) 0.2021(2) 0.0195(5) Uani 1 1 d . . . . .
O3 O 0.0916(3) 0.2282(3) 0.4021(2) 0.0324(6) Uani 1 1 d . . . . .
O4 O 0.1186(3) 0.8939(3) 0.1183(2) 0.0331(6) Uani 1 1 d . . . . .
C1 C 0.1681(4) 0.3143(3) 0.3934(3) 0.0207(7) Uani 1 1 d . . . . .
C2 C 0.2697(4) 0.3032(3) 0.4809(3) 0.0196(7) Uani 1 1 d . . . . .
C15 C 0.5904(4) 0.6954(3) 0.1552(3) 0.0199(7) Uani 1 1 d . . . . .
C12 C 0.2791(4) 0.8625(3) 0.2526(3) 0.0241(7) Uani 1 1 d . . . . .
C3 C 0.3388(4) 0.1558(3) 0.5161(3) 0.0253(7) Uani 1 1 d . . . . .
H3A H 0.4080 0.1532 0.5652 0.038 Uiso 1 1 calc R U . . .
H3B H 0.3968 0.1108 0.4469 0.038 Uiso 1 1 calc R U . . .
H3C H 0.2550 0.1106 0.5583 0.038 Uiso 1 1 calc R U . . .
C4 C 0.1698(4) 0.3788(4) 0.5868(3) 0.0273(8) Uani 1 1 d . . . . .
H4A H 0.1273 0.4704 0.5609 0.041 Uiso 1 1 calc R U . . .
H4B H 0.2340 0.3796 0.6389 0.041 Uiso 1 1 calc R U . . .
H4C H 0.0851 0.3339 0.6273 0.041 Uiso 1 1 calc R U . . .
C5 C 0.5722(4) 0.2955(3) 0.3131(3) 0.0205(7) Uani 1 1 d . . . . .
C6 C 0.5393(4) 0.2532(3) 0.2194(3) 0.0247(7) Uani 1 1 d . . . . .
H6 H 0.4382 0.2787 0.2077 0.030 Uiso 1 1 calc R U . . .
C11 C 0.1851(4) 0.8129(3) 0.1830(3) 0.0218(7) Uani 1 1 d . . . . .
C16 C 0.6006(4) 0.6009(4) 0.0793(3) 0.0273(8) Uani 1 1 d . . . . .
H16 H 0.5199 0.5541 0.0910 0.033 Uiso 1 1 calc R U . . .
C17 C 0.7315(5) 0.5768(4) -0.0138(3) 0.0352(9) Uani 1 1 d . . . . .
H17 H 0.7404 0.5113 -0.0635 0.042 Uiso 1 1 calc R U . . .
C10 C 0.7248(4) 0.2603(4) 0.3293(3) 0.0314(8) Uani 1 1 d . . . . .
H10 H 0.7472 0.2898 0.3920 0.038 Uiso 1 1 calc R U . . .
C14 C 0.3489(5) 0.9824(4) 0.1879(4) 0.0325(9) Uani 1 1 d . . . . .
H14A H 0.2660 1.0559 0.1725 0.049 Uiso 1 1 calc R U . . .
H14B H 0.4210 0.9563 0.1150 0.049 Uiso 1 1 calc R U . . .
H14C H 0.4040 1.0111 0.2353 0.049 Uiso 1 1 calc R U . . .
C7 C 0.6579(4) 0.1726(4) 0.1428(3) 0.0306(8) Uani 1 1 d . . . . .
H7 H 0.6359 0.1429 0.0801 0.037 Uiso 1 1 calc R U . . .
C20 C 0.7094(4) 0.7671(4) 0.1377(3) 0.0307(8) Uani 1 1 d . . . . .
H20 H 0.7022 0.8298 0.1894 0.037 Uiso 1 1 calc R U . . .
C19 C 0.8389(5) 0.7442(5) 0.0423(4) 0.0406(10) Uani 1 1 d . . . . .
H19 H 0.9185 0.7926 0.0293 0.049 Uiso 1 1 calc R U . . .
C13 C 0.1697(4) 0.8957(4) 0.3739(3) 0.0296(8) Uani 1 1 d . . . . .
H13A H 0.2285 0.9196 0.4210 0.044 Uiso 1 1 calc R U . . .
H13B H 0.1273 0.8178 0.4119 0.044 Uiso 1 1 calc R U . . .
H13C H 0.0850 0.9705 0.3644 0.044 Uiso 1 1 calc R U . . .
C8 C 0.8087(4) 0.1357(4) 0.1589(4) 0.0356(9) Uani 1 1 d . . . . .
H8 H 0.8874 0.0807 0.1076 0.043 Uiso 1 1 calc R U . . .
C18 C 0.8500(5) 0.6491(4) -0.0340(4) 0.0373(9) Uani 1 1 d . . . . .
H18 H 0.9364 0.6342 -0.0982 0.045 Uiso 1 1 calc R U . . .
C9 C 0.8426(4) 0.1805(4) 0.2508(4) 0.0391(10) Uani 1 1 d . . . . .
H9 H 0.9448 0.1573 0.2603 0.047 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O1 2.021(2) . ?
Pd1 O2 2.024(2) . ?
Pd1 S1 2.2538(8) . ?
Pd1 S2 2.2616(8) . ?
S1 C5 1.779(3) . ?
S1 C2 1.853(3) . ?
S2 C15 1.795(3) . ?
S2 C12 1.858(3) . ?
O1 C1 1.290(4) . ?
O2 C11 1.292(4) . ?
O3 C1 1.215(4) . ?
O4 C11 1.210(4) . ?
C1 C2 1.543(4) . ?
C2 C4 1.525(5) . ?
C2 C3 1.527(4) . ?
C15 C16 1.385(5) . ?
C15 C20 1.389(5) . ?
C12 C14 1.516(5) . ?
C12 C13 1.541(5) . ?
C12 C11 1.541(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.379(5) . ?
C5 C10 1.398(5) . ?
C6 C7 1.385(5) . ?
C6 H6 0.9300 . ?
C16 C17 1.380(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.386(6) . ?
C17 H17 0.9300 . ?
C10 C9 1.390(6) . ?
C10 H10 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C7 C8 1.382(5) . ?
C7 H7 0.9300 . ?
C20 C19 1.388(5) . ?
C20 H20 0.9300 . ?
C19 C18 1.391(6) . ?
C19 H19 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C8 C9 1.376(6) . ?
C8 H8 0.9300 . ?
C18 H18 0.9300 . ?
C9 H9 0.9300 . ?

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
O1 Pd1 O2 90.77(9) . . ?
O1 Pd1 S1 85.73(6) . . ?
O2 Pd1 S1 176.21(6) . . ?
O1 Pd1 S2 176.47(6) . . ?
O2 Pd1 S2 85.73(7) . . ?
S1 Pd1 S2 97.78(3) . . ?
C5 S1 C2 105.68(15) . . ?
C5 S1 Pd1 103.70(11) . . ?
C2 S1 Pd1 96.44(11) . . ?
C15 S2 C12 107.27(16) . . ?
C15 S2 Pd1 106.46(11) . . ?
C12 S2 Pd1 95.59(11) . . ?
C1 O1 Pd1 120.7(2) . . ?
C11 O2 Pd1 120.3(2) . . ?
O3 C1 O1 122.8(3) . . ?
O3 C1 C2 119.0(3) . . ?
O1 C1 C2 118.2(3) . . ?
C4 C2 C3 112.1(3) . . ?
C4 C2 C1 108.5(3) . . ?
C3 C2 C1 111.9(3) . . ?
C4 C2 S1 103.7(2) . . ?
C3 C2 S1 110.4(2) . . ?
C1 C2 S1 109.9(2) . . ?
C16 C15 C20 120.8(3) . . ?
C16 C15 S2 122.3(3) . . ?
C20 C15 S2 116.6(3) . . ?
C14 C12 C13 111.9(3) . . ?
C14 C12 C11 112.4(3) . . ?
C13 C12 C11 108.2(3) . . ?
C14 C12 S2 110.8(3) . . ?
C13 C12 S2 103.7(2) . . ?
C11 C12 S2 109.4(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 120.5(3) . . ?
C6 C5 S1 123.3(2) . . ?
C10 C5 S1 116.2(3) . . ?
C5 C6 C7 119.5(3) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
O4 C11 O2 122.8(3) . . ?
O4 C11 C12 119.2(3) . . ?
O2 C11 C12 117.9(3) . . ?
C17 C16 C15 119.4(3) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C16 C17 C18 120.6(4) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C9 C10 C5 119.2(4) . . ?
C9 C10 H10 120.4 . . ?
C5 C10 H10 120.4 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C7 C6 120.5(4) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C19 C20 C15 119.3(3) . . ?
C19 C20 H20 120.3 . . ?
C15 C20 H20 120.3 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C17 C18 C19 119.7(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C8 C9 C10 120.3(3) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?

_refine_diff_density_max         0.700
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.082



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_molan472_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 1969711'
loop_
_audit_author_name
_audit_author_address
'Edwin Otten'
;University of Groningen
Netherlands
;
_audit_update_record             
;
2019-12-03 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H29 O4 P Pd S'
_chemical_formula_weight         622.96

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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1765(4)
_cell_length_b                   28.3513(11)
_cell_length_c                   9.7423(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.9510(10)
_cell_angle_gamma                90
_cell_volume                     2688.70(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2.93
_cell_measurement_theta_max      26.38

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.862
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35241
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.925
_diffrn_reflns_theta_max         26.456
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5489
_reflns_number_gt                4609
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0082P)²+8.6315P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5489
_refine_ls_number_parameters     337
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.0852
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.68118(3) 0.64725(2) 0.66767(3) 0.01749(8) Uani 1 1 d . . . . .
S1 S 0.51163(9) 0.68207(3) 0.49354(10) 0.0205(2) Uani 1 1 d . . . . .
P1 P 0.80600(10) 0.62969(3) 0.51947(10) 0.0177(2) Uani 1 1 d . . . . .
O1 O 0.5622(3) 0.66142(10) 0.8006(3) 0.0258(6) Uani 1 1 d . . . . .
O2 O 0.3730(3) 0.69511(11) 0.8232(3) 0.0366(7) Uani 1 1 d . . . . .
O3 O 0.8240(3) 0.61906(9) 0.8402(3) 0.0203(5) Uani 1 1 d . . . . .
O4 O 0.7013(3) 0.55316(10) 0.7732(3) 0.0273(6) Uani 1 1 d . . . . .
C1 C 0.4576(4) 0.68881(14) 0.7570(4) 0.0272(9) Uani 1 1 d . . . . .
C2 C 0.4411(4) 0.71682(14) 0.6177(4) 0.0244(9) Uani 1 1 d . . . . .
C3 C 0.5349(4) 0.76074(15) 0.6502(5) 0.0308(10) Uani 1 1 d . . . . .
H3A H 0.5120 0.7800 0.7236 0.046 Uiso 1 1 calc R U . . .
H3B H 0.5211 0.7794 0.5624 0.046 Uiso 1 1 calc R U . . .
H3C H 0.6311 0.7507 0.6851 0.046 Uiso 1 1 calc R U . . .
C30 C 0.8892(4) 0.55337(15) 0.9900(4) 0.0292(9) Uani 1 1 d . . . . .
H30A H 0.8520 0.5228 1.0074 0.044 Uiso 1 1 calc R U . . .
H30B H 0.8969 0.5742 1.0722 0.044 Uiso 1 1 calc R U . . .
H30C H 0.9802 0.5488 0.9768 0.044 Uiso 1 1 calc R U . . .
C29 C 0.7943(4) 0.57544(14) 0.8565(4) 0.0200(8) Uani 1 1 d . . . . .
C4 C 0.2925(4) 0.73009(15) 0.5440(5) 0.0313(10) Uani 1 1 d . . . . .
H4A H 0.2580 0.7500 0.6082 0.047 Uiso 1 1 calc R U . . .
H4B H 0.2367 0.7014 0.5207 0.047 Uiso 1 1 calc R U . . .
H4C H 0.2871 0.7475 0.4556 0.047 Uiso 1 1 calc R U . . .
C5 C 0.3878(4) 0.63702(13) 0.4242(4) 0.0199(8) Uani 1 1 d . . . . .
C6 C 0.3603(4) 0.60129(13) 0.5088(4) 0.0208(8) Uani 1 1 d . . . . .
H6 H 0.4055 0.6006 0.6090 0.025 Uiso 1 1 calc R U . . .
C7 C 0.2664(4) 0.56673(14) 0.4460(4) 0.0244(9) Uani 1 1 d . . . . .
H7 H 0.2460 0.5423 0.5034 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2016(4) 0.56743(15) 0.2990(4) 0.0260(9) Uani 1 1 d . . . . .
H8 H 0.1376 0.5434 0.2565 0.031 Uiso 1 1 calc R U . . .
C9 C 0.2300(4) 0.60291(16) 0.2145(4) 0.0324(10) Uani 1 1 d . . . . .
H9 H 0.1864 0.6032 0.1139 0.039 Uiso 1 1 calc R U . . .
C10 C 0.3225(4) 0.63802(15) 0.2775(4) 0.0278(9) Uani 1 1 d . . . . .
H10 H 0.3413 0.6628 0.2204 0.033 Uiso 1 1 calc R U . . .
C11 C 0.7000(4) 0.59502(14) 0.3708(4) 0.0209(8) Uani 1 1 d . . . . .
C12 C 0.6300(4) 0.55644(14) 0.4053(4) 0.0211(8) Uani 1 1 d . . . . .
H12 H 0.6441 0.5479 0.5029 0.025 Uiso 1 1 calc R U . . .
C13 C 0.5397(4) 0.53049(15) 0.2966(5) 0.0274(9) Uani 1 1 d . . . . .
H13 H 0.4935 0.5039 0.3200 0.033 Uiso 1 1 calc R U . . .
C14 C 0.5172(4) 0.54335(17) 0.1551(5) 0.0351(11) Uani 1 1 d . . . . .
H14 H 0.4553 0.5256 0.0814 0.042 Uiso 1 1 calc R U . . .
C15 C 0.5840(4) 0.58173(19) 0.1198(4) 0.0384(12) Uani 1 1 d . . . . .
H15 H 0.5675 0.5904 0.0221 0.046 Uiso 1 1 calc R U . . .
C17 C 0.9607(4) 0.59662(13) 0.6097(4) 0.0186(8) Uani 1 1 d . . . . .
C16 C 0.6761(4) 0.60795(16) 0.2277(4) 0.0284(9) Uani 1 1 d . . . . .
H16 H 0.7221 0.6344 0.2034 0.034 Uiso 1 1 calc R U . . .
C18 C 0.9627(4) 0.54789(14) 0.6128(4) 0.0226(8) Uani 1 1 d . . . . .
H18 H 0.8854 0.5305 0.5580 0.027 Uiso 1 1 calc R U . . .
C19 C 1.0784(4) 0.52449(15) 0.6967(4) 0.0243(9) Uani 1 1 d . . . . .
H19 H 1.0802 0.4910 0.6977 0.029 Uiso 1 1 calc R U . . .
C20 C 1.1910(4) 0.54933(15) 0.7787(4) 0.0259(9) Uani 1 1 d . . . . .
H20 H 1.2686 0.5329 0.8373 0.031 Uiso 1 1 calc R U . . .
C21 C 1.1906(4) 0.59782(15) 0.7754(4) 0.0263(9) Uani 1 1 d . . . . .
H21 H 1.2682 0.6150 0.8305 0.032 Uiso 1 1 calc R U . . .
C22 C 1.0751(4) 0.62161(14) 0.6902(4) 0.0237(8) Uani 1 1 d . . . . .
H22 H 1.0747 0.6551 0.6872 0.028 Uiso 1 1 calc R U . . .
C23 C 0.8683(4) 0.67973(16) 0.4414(5) 0.0324(11) Uani 1 1 d . . . . .
C24 C 0.8351(5) 0.72485(16) 0.4722(5) 0.0422(13) Uani 1 1 d . . . . .
H24 H 0.7778 0.7296 0.5326 0.051 Uiso 1 1 calc R U . . .
C25 C 0.8856(6) 0.7636(2) 0.4147(7) 0.069(2) Uani 1 1 d . . . . .
H25 H 0.8641 0.7947 0.4372 0.082 Uiso 1 1 calc R U . . .
C26 C 0.9659(7) 0.7566(3) 0.3261(8) 0.094(3) Uani 1 1 d . . . . .
H26 H 0.9994 0.7830 0.2862 0.112 Uiso 1 1 calc R U . . .
C27 C 0.9986(5) 0.7120(3) 0.2945(7) 0.082(3) Uani 1 1 d . . . . .
H27 H 1.0537 0.7077 0.2318 0.098 Uiso 1 1 calc R U . . .
C28 C 0.9520(4) 0.6726(2) 0.3531(5) 0.0480(14) Uani 1 1 d . . . . .
H28 H 0.9771 0.6417 0.3330 0.058 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O3 2.038(2) . ?
Pd1 O1 2.054(3) . ?
Pd1 P1 2.2396(10) . ?
Pd1 S1 2.2633(9) . ?
S1 C5 1.783(4) . ?
S1 C2 1.859(4) . ?
P1 C23 1.809(4) . ?
P1 C11 1.821(4) . ?
P1 C17 1.823(4) . ?
O1 C1 1.286(5) . ?
O2 C1 1.230(5) . ?
O3 C29 1.294(5) . ?
O4 C29 1.227(5) . ?
C1 C2 1.538(6) . ?
C2 C4 1.519(5) . ?
C2 C3 1.545(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C30 C29 1.511(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.385(5) . ?
C5 C10 1.390(5) . ?
C6 C7 1.381(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.382(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C16 1.392(5) . ?
C11 C12 1.399(5) . ?
C12 C13 1.393(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.401(6) . ?
C15 H15 0.9500 . ?
C17 C18 1.382(5) . ?
C17 C22 1.392(5) . ?
C16 H16 0.9500 . ?
C18 C19 1.391(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.375(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.399(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.379(7) . ?
C23 C28 1.391(7) . ?
C24 C25 1.398(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.366(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.364(12) . ?
C26 H26 0.9500 . ?
C27 C28 1.399(7) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?

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
O3 Pd1 O1 88.10(10) . . ?
O3 Pd1 P1 92.41(8) . . ?
O1 Pd1 P1 177.98(8) . . ?
O3 Pd1 S1 173.69(8) . . ?
O1 Pd1 S1 85.78(8) . . ?
P1 Pd1 S1 93.75(4) . . ?
C5 S1 C2 105.16(18) . . ?
C5 S1 Pd1 105.77(13) . . ?
C2 S1 Pd1 95.62(13) . . ?
C23 P1 C11 106.71(19) . . ?
C23 P1 C17 104.27(18) . . ?
C11 P1 C17 109.51(17) . . ?
C23 P1 Pd1 115.52(17) . . ?
C11 P1 Pd1 108.49(12) . . ?
C17 P1 Pd1 112.08(12) . . ?
C1 O1 Pd1 119.6(3) . . ?
C29 O3 Pd1 109.9(2) . . ?
O2 C1 O1 123.6(4) . . ?
O2 C1 C2 118.3(4) . . ?
O1 C1 C2 118.1(4) . . ?
C4 C2 C1 112.5(4) . . ?
C4 C2 C3 111.6(3) . . ?
C1 C2 C3 109.5(3) . . ?
C4 C2 S1 110.1(3) . . ?
C1 C2 S1 109.7(3) . . ?
C3 C2 S1 103.1(3) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O4 C29 O3 125.0(3) . . ?
O4 C29 C30 122.2(4) . . ?
O3 C29 C30 112.8(3) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 120.5(3) . . ?
C6 C5 S1 122.8(3) . . ?
C10 C5 S1 116.6(3) . . ?
C7 C6 C5 119.3(4) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C8 120.4(4) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 120.3(4) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 119.4(4) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C5 120.1(4) . . ?
C9 C10 H10 120.0 . . ?
C5 C10 H10 120.0 . . ?
C16 C11 C12 119.6(4) . . ?
C16 C11 P1 123.0(3) . . ?
C12 C11 P1 117.1(3) . . ?
C13 C12 C11 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.5(4) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 120.2(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C18 C17 C22 119.5(3) . . ?
C18 C17 P1 122.0(3) . . ?
C22 C17 P1 118.2(3) . . ?
C11 C16 C15 119.7(4) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 120.9(4) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 119.5(4) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C17 C22 C21 120.6(4) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C28 120.2(4) . . ?
C24 C23 P1 119.8(4) . . ?
C28 C23 P1 120.0(4) . . ?
C23 C24 C25 120.0(6) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C26 C25 C24 119.8(7) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C27 C26 C25 120.5(5) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 120.9(7) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C27 118.6(6) . . ?
C23 C28 H28 120.7 . . ?
C27 C28 H28 120.7 . . ?

_refine_diff_density_max         0.924
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.094



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_molan488_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1969712'
loop_
_audit_author_name
_audit_author_address
'Edwin Otten'
;University of Groningen
Netherlands
;
_audit_update_record             
;
2019-12-03 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H31 O2 P Pd S'
_chemical_formula_weight         641.02

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'
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'
S S 0.1246 0.1234 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

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'

_cell_length_a                   9.7129(4)
_cell_length_b                   11.8850(4)
_cell_length_c                   24.9669(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2882.12(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9714
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      29.64

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.802
_shelx_estimated_absorpt_T_min   0.778
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53234
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.988
_diffrn_reflns_theta_max         29.634
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8114
_reflns_number_gt                7914
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0184P)²+0.7461P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3418 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(4)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         8114
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0163
_refine_ls_wR_factor_ref         0.0392
_refine_ls_wR_factor_gt          0.0389
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.71383(2) 0.59114(2) 0.62310(2) 0.00925(3) Uani 1 1 d . . . . .
S1 S 0.78422(5) 0.73320(3) 0.68259(2) 0.01271(8) Uani 1 1 d . . . . .
P1 P 0.61045(5) 0.46114(4) 0.56965(2) 0.00927(8) Uani 1 1 d . . . . .
O1 O 0.82170(14) 0.48428(11) 0.67582(5) 0.0141(3) Uani 1 1 d . . . . .
O2 O 0.92870(18) 0.46602(12) 0.75401(6) 0.0238(3) Uani 1 1 d . . . . .
C1 C 0.6177(2) 0.70700(15) 0.57907(7) 0.0119(3) Uani 1 1 d . . . . .
C2 C 0.4805(2) 0.73743(17) 0.58759(8) 0.0155(4) Uani 1 1 d . . . . .
H2 H 0.4284 0.7008 0.6147 0.019 Uiso 1 1 calc R U . . .
C3 C 0.4196(2) 0.82147(17) 0.55649(9) 0.0205(4) Uani 1 1 d . . . . .
H3 H 0.3266 0.8424 0.5628 0.025 Uiso 1 1 calc R U . . .
C4 C 0.4943(2) 0.87469(17) 0.51633(9) 0.0226(4) Uani 1 1 d . . . . .
H4 H 0.4518 0.9302 0.4945 0.027 Uiso 1 1 calc R U . . .
C5 C 0.6318(2) 0.84616(17) 0.50830(8) 0.0197(4) Uani 1 1 d . . . . .
H5 H 0.6838 0.8829 0.4812 0.024 Uiso 1 1 calc R U . . .
C6 C 0.69307(19) 0.76373(15) 0.53997(7) 0.0146(3) Uani 1 1 d . . . . .
H6 H 0.7875 0.7459 0.5349 0.018 Uiso 1 1 calc R U . . .
C7 C 0.8857(2) 0.52380(16) 0.71661(7) 0.0136(3) Uani 1 1 d . . . . .
C8 C 0.9178(2) 0.65209(16) 0.71799(8) 0.0140(4) Uani 1 1 d . . . . .
C9 C 1.0474(2) 0.67263(17) 0.68397(9) 0.0203(4) Uani 1 1 d . . . . .
H9A H 1.1241 0.6286 0.6985 0.030 Uiso 1 1 calc R U . . .
H9B H 1.0709 0.7528 0.6848 0.030 Uiso 1 1 calc R U . . .
H9C H 1.0297 0.6495 0.6469 0.030 Uiso 1 1 calc R U . . .
C10 C 0.9409(3) 0.69775(18) 0.77429(8) 0.0221(4) Uani 1 1 d . . . . .
H10A H 1.0157 0.6559 0.7915 0.033 Uiso 1 1 calc R U . . .
H10B H 0.8563 0.6891 0.7953 0.033 Uiso 1 1 calc R U . . .
H10C H 0.9655 0.7776 0.7723 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6327(2) 0.73117(17) 0.72308(8) 0.0172(4) Uani 1 1 d . . . . .
C12 C 0.5997(3) 0.6439(2) 0.75755(11) 0.0343(6) Uani 1 1 d . . . . .
H12 H 0.6615 0.5828 0.7623 0.041 Uiso 1 1 calc R U . . .
C13 C 0.4743(3) 0.6467(2) 0.78531(13) 0.0449(8) Uani 1 1 d . . . . .
H13 H 0.4519 0.5877 0.8095 0.054 Uiso 1 1 calc R U . . .
C14 C 0.3829(3) 0.7345(2) 0.77785(11) 0.0361(6) Uani 1 1 d . . . . .
H14 H 0.2978 0.7359 0.7966 0.043 Uiso 1 1 calc R U . . .
C15 C 0.4160(3) 0.8190(3) 0.74330(11) 0.0367(6) Uani 1 1 d . . . . .
H15 H 0.3526 0.8788 0.7376 0.044 Uiso 1 1 calc R U . . .
C16 C 0.5414(2) 0.8192(2) 0.71610(10) 0.0273(5) Uani 1 1 d . . . . .
H16 H 0.5641 0.8797 0.6928 0.033 Uiso 1 1 calc R U . . .
C17 C 0.43019(19) 0.44803(15) 0.58872(7) 0.0111(3) Uani 1 1 d . . . . .
C18 C 0.40104(19) 0.45520(17) 0.64365(7) 0.0146(4) Uani 1 1 d . . . . .
H18 H 0.4717 0.4757 0.6681 0.018 Uiso 1 1 calc R U . . .
C19 C 0.2696(2) 0.43246(16) 0.66249(7) 0.0171(4) Uani 1 1 d . . . . .
H19 H 0.2510 0.4361 0.6998 0.021 Uiso 1 1 calc R U . . .
C20 C 0.16502(17) 0.40424(17) 0.62680(8) 0.0169(3) Uani 1 1 d . . . . .
H20 H 0.0748 0.3896 0.6397 0.020 Uiso 1 1 calc R U . . .
C21 C 0.19268(17) 0.39753(16) 0.57234(7) 0.0157(3) Uani 1 1 d . . . . .
H21 H 0.1212 0.3784 0.5480 0.019 Uiso 1 1 calc R U . . .
C22 C 0.32548(17) 0.41892(16) 0.55320(7) 0.0129(3) Uani 1 1 d . . . . .
H22 H 0.3443 0.4136 0.5159 0.015 Uiso 1 1 calc R U . . .
C23 C 0.61581(18) 0.48033(15) 0.49720(7) 0.0113(3) Uani 1 1 d . . . . .
C24 C 0.53789(19) 0.56532(15) 0.47271(7) 0.0132(3) Uani 1 1 d . . . . .
H24 H 0.4794 0.6117 0.4938 0.016 Uiso 1 1 calc R U . . .
C25 C 0.54598(19) 0.58193(17) 0.41758(7) 0.0159(3) Uani 1 1 d . . . . .
H25 H 0.4924 0.6394 0.4013 0.019 Uiso 1 1 calc R U . . .
C26 C 0.6316(2) 0.51547(17) 0.38601(7) 0.0177(4) Uani 1 1 d . . . . .
H26 H 0.6365 0.5272 0.3484 0.021 Uiso 1 1 calc R U . . .
C27 C 0.7099(2) 0.43162(15) 0.41018(7) 0.0170(3) Uani 1 1 d . . . . .
H27 H 0.7690 0.3861 0.3890 0.020 Uiso 1 1 calc R U . . .
C28 C 0.70214(18) 0.41393(16) 0.46536(7) 0.0140(3) Uani 1 1 d . . . . .
H28 H 0.7559 0.3563 0.4814 0.017 Uiso 1 1 calc R U . . .
C29 C 0.67175(19) 0.31760(15) 0.57890(7) 0.0119(3) Uani 1 1 d . . . . .
C30 C 0.81056(19) 0.29867(16) 0.59005(7) 0.0155(4) Uani 1 1 d . . . . .
H30 H 0.8723 0.3604 0.5926 0.019 Uiso 1 1 calc R U . . .
C31 C 0.8587(2) 0.18940(18) 0.59746(8) 0.0201(4) Uani 1 1 d . . . . .
H31 H 0.9534 0.1767 0.6049 0.024 Uiso 1 1 calc R U . . .
C32 C 0.7691(2) 0.09938(18) 0.59407(8) 0.0223(4) Uani 1 1 d . . . . .
H32 H 0.8019 0.0251 0.6000 0.027 Uiso 1 1 calc R U . . .
C33 C 0.6309(2) 0.11727(17) 0.58205(9) 0.0221(4) Uani 1 1 d . . . . .
H33 H 0.5698 0.0551 0.5790 0.026 Uiso 1 1 calc R U . . .
C34 C 0.5824(2) 0.22576(17) 0.57448(8) 0.0178(4) Uani 1 1 d . . . . .
H34 H 0.4880 0.2378 0.5663 0.021 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C1 1.9938(19) . ?
Pd1 O1 2.1079(13) . ?
Pd1 P1 2.2752(5) . ?
Pd1 S1 2.3502(4) . ?
S1 C11 1.786(2) . ?
S1 C8 1.8424(19) . ?
P1 C17 1.8211(19) . ?
P1 C29 1.8216(19) . ?
P1 C23 1.8240(18) . ?
O1 C7 1.282(2) . ?
O2 C7 1.232(2) . ?
C1 C6 1.394(3) . ?
C1 C2 1.398(3) . ?
C2 C3 1.397(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.557(2) . ?
C8 C10 1.523(3) . ?
C8 C9 1.538(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C16 1.382(3) . ?
C11 C12 1.385(3) . ?
C12 C13 1.402(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.363(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.395(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.393(2) . ?
C17 C18 1.403(3) . ?
C18 C19 1.387(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.392(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.388(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.399(2) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.399(3) . ?
C23 C24 1.402(3) . ?
C24 C25 1.393(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.392(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.391(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.395(2) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.395(3) . ?
C29 C34 1.399(3) . ?
C30 C31 1.393(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.386(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

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
C1 Pd1 O1 173.23(6) . . ?
C1 Pd1 P1 86.50(5) . . ?
O1 Pd1 P1 100.16(4) . . ?
C1 Pd1 S1 89.34(5) . . ?
O1 Pd1 S1 83.90(4) . . ?
P1 Pd1 S1 170.706(18) . . ?
C11 S1 C8 107.56(9) . . ?
C11 S1 Pd1 96.22(6) . . ?
C8 S1 Pd1 97.60(6) . . ?
C17 P1 C29 101.59(8) . . ?
C17 P1 C23 107.30(8) . . ?
C29 P1 C23 103.50(8) . . ?
C17 P1 Pd1 109.22(6) . . ?
C29 P1 Pd1 114.67(6) . . ?
C23 P1 Pd1 118.96(6) . . ?
C7 O1 Pd1 121.07(12) . . ?
C6 C1 C2 118.82(18) . . ?
C6 C1 Pd1 118.33(14) . . ?
C2 C1 Pd1 122.77(15) . . ?
C3 C2 C1 120.30(19) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 120.34(19) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.61(19) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 119.96(19) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 120.91(18) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O2 C7 O1 124.21(18) . . ?
O2 C7 C8 117.45(17) . . ?
O1 C7 C8 118.27(16) . . ?
C10 C8 C9 109.43(17) . . ?
C10 C8 C7 113.51(16) . . ?
C9 C8 C7 107.90(16) . . ?
C10 C8 S1 111.10(14) . . ?
C9 C8 S1 103.21(13) . . ?
C7 C8 S1 111.14(13) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 119.8(2) . . ?
C16 C11 S1 116.54(17) . . ?
C12 C11 S1 123.55(17) . . ?
C11 C12 C13 119.4(2) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 121.0(2) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 119.8(2) . . ?
C11 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C22 C17 C18 119.35(16) . . ?
C22 C17 P1 123.83(14) . . ?
C18 C17 P1 116.38(14) . . ?
C19 C18 C17 120.36(17) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 120.09(17) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 119.96(16) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.17(16) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C17 C22 C21 120.06(16) . . ?
C17 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C28 C23 C24 118.81(16) . . ?
C28 C23 P1 120.67(14) . . ?
C24 C23 P1 120.46(14) . . ?
C25 C24 C23 120.16(17) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 120.87(18) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C27 C26 C25 119.17(17) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 C28 120.44(18) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C23 120.54(18) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
C30 C29 C34 119.32(17) . . ?
C30 C29 P1 119.49(14) . . ?
C34 C29 P1 121.19(14) . . ?
C31 C30 C29 120.11(19) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C32 C31 C30 120.15(19) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 120.17(19) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 120.0(2) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C29 120.28(19) . . ?
C33 C34 H34 119.9 . . ?
C29 C34 H34 119.9 . . ?

_refine_diff_density_max         0.293
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.051



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_molan488a_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 1969713'
loop_
_audit_author_name
_audit_author_address
'Edwin Otten'
;University of Groningen
Netherlands
;
_audit_update_record             
;
2019-12-03 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H31 O2 P Pd S'
_chemical_formula_weight         641.02

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'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

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'

_cell_length_a                   9.6976(5)
_cell_length_b                   11.8942(7)
_cell_length_c                   24.9749(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2880.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9828
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.13

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_min          0.06
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_max          0.12
_exptl_absorpt_coefficient_mu    0.802
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55231
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.987
_diffrn_reflns_theta_max         27.194
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6397
_reflns_number_gt                6239
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²+0.9379P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(4)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         6397
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0155
_refine_ls_wR_factor_ref         0.0385
_refine_ls_wR_factor_gt          0.0380
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.71395(2) 0.59110(2) 0.37690(2) 0.00973(4) Uani 1 1 d . . . . .
S1 S 0.78435(6) 0.73310(4) 0.31740(2) 0.01323(10) Uani 1 1 d . . . . .
P1 P 0.61053(5) 0.46120(5) 0.43035(2) 0.00965(10) Uani 1 1 d . . . . .
O1 O 0.82182(16) 0.48411(13) 0.32422(6) 0.0143(3) Uani 1 1 d . . . . .
O2 O 0.9289(2) 0.46596(14) 0.24599(7) 0.0241(4) Uani 1 1 d . . . . .
C1 C 0.6178(2) 0.70694(18) 0.42103(9) 0.0124(4) Uani 1 1 d . . . . .
C2 C 0.4806(2) 0.7374(2) 0.41242(9) 0.0159(4) Uani 1 1 d . . . . .
H2 H 0.4284 0.7009 0.3853 0.019 Uiso 1 1 calc R U . . .
C3 C 0.4198(2) 0.8214(2) 0.44356(10) 0.0212(5) Uani 1 1 d . . . . .
H3 H 0.3267 0.8424 0.4372 0.025 Uiso 1 1 calc R U . . .
C4 C 0.4943(3) 0.8744(2) 0.48367(10) 0.0228(5) Uani 1 1 d . . . . .
H4 H 0.4517 0.9297 0.5056 0.027 Uiso 1 1 calc R U . . .
C5 C 0.6317(3) 0.8460(2) 0.49159(10) 0.0204(5) Uani 1 1 d . . . . .
H5 H 0.6838 0.8830 0.5186 0.024 Uiso 1 1 calc R U . . .
C6 C 0.6932(2) 0.76375(18) 0.46017(9) 0.0149(4) Uani 1 1 d . . . . .
H6 H 0.7878 0.7459 0.4654 0.018 Uiso 1 1 calc R U . . .
C7 C 0.8858(2) 0.52379(18) 0.28333(9) 0.0136(4) Uani 1 1 d . . . . .
C8 C 0.9179(2) 0.65220(19) 0.28195(9) 0.0148(4) Uani 1 1 d . . . . .
C9 C 1.0479(2) 0.6727(2) 0.31596(10) 0.0210(5) Uani 1 1 d . . . . .
H9A H 1.1248 0.6289 0.3013 0.032 Uiso 1 1 calc R U . . .
H9B H 1.0303 0.6494 0.3530 0.032 Uiso 1 1 calc R U . . .
H9C H 1.0713 0.7528 0.3152 0.032 Uiso 1 1 calc R U . . .
C10 C 0.9410(3) 0.6977(2) 0.22564(10) 0.0225(5) Uani 1 1 d . . . . .
H10A H 1.0146 0.6548 0.2082 0.034 Uiso 1 1 calc R U . . .
H10B H 0.9674 0.7771 0.2276 0.034 Uiso 1 1 calc R U . . .
H10C H 0.8557 0.6904 0.2049 0.034 Uiso 1 1 calc R U . . .
C11 C 0.6326(2) 0.7309(2) 0.27693(9) 0.0177(5) Uani 1 1 d . . . . .
C12 C 0.5414(3) 0.8191(2) 0.28377(11) 0.0282(6) Uani 1 1 d . . . . .
H12 H 0.5643 0.8797 0.3069 0.034 Uiso 1 1 calc R U . . .
C13 C 0.4161(3) 0.8190(3) 0.25660(12) 0.0367(7) Uani 1 1 d . . . . .
H13 H 0.3528 0.8788 0.2622 0.044 Uiso 1 1 calc R U . . .
C14 C 0.3829(3) 0.7343(3) 0.22212(12) 0.0360(7) Uani 1 1 d . . . . .
H14 H 0.2976 0.7356 0.2034 0.043 Uiso 1 1 calc R U . . .
C15 C 0.4743(4) 0.6466(3) 0.21461(14) 0.0454(9) Uani 1 1 d . . . . .
H15 H 0.4521 0.5878 0.1904 0.054 Uiso 1 1 calc R U . . .
C16 C 0.5993(3) 0.6439(2) 0.24245(12) 0.0347(7) Uani 1 1 d . . . . .
H16 H 0.6611 0.5827 0.2377 0.042 Uiso 1 1 calc R U . . .
C17 C 0.6717(2) 0.31772(18) 0.42124(8) 0.0125(4) Uani 1 1 d . . . . .
C18 C 0.5824(2) 0.2257(2) 0.42552(9) 0.0177(5) Uani 1 1 d . . . . .
H18 H 0.4879 0.2378 0.4337 0.021 Uiso 1 1 calc R U . . .
C19 C 0.6307(3) 0.1172(2) 0.41795(10) 0.0224(5) Uani 1 1 d . . . . .
H19 H 0.5693 0.0552 0.4209 0.027 Uiso 1 1 calc R U . . .
C20 C 0.7691(3) 0.0992(2) 0.40601(9) 0.0227(5) Uani 1 1 d . . . . .
H20 H 0.8020 0.0250 0.4002 0.027 Uiso 1 1 calc R U . . .
C21 C 0.8586(3) 0.1894(2) 0.40260(9) 0.0206(5) Uani 1 1 d . . . . .
H21 H 0.9534 0.1768 0.3952 0.025 Uiso 1 1 calc R U . . .
C22 C 0.8105(2) 0.29852(19) 0.40987(9) 0.0158(5) Uani 1 1 d . . . . .
H22 H 0.8724 0.3602 0.4071 0.019 Uiso 1 1 calc R U . . .
C23 C 0.6158(2) 0.48036(18) 0.50283(8) 0.0121(4) Uani 1 1 d . . . . .
C24 C 0.5380(2) 0.56556(18) 0.52730(9) 0.0140(4) Uani 1 1 d . . . . .
H24 H 0.4798 0.6122 0.5062 0.017 Uiso 1 1 calc R U . . .
C25 C 0.5461(2) 0.5819(2) 0.58236(9) 0.0166(4) Uani 1 1 d . . . . .
H25 H 0.4923 0.6392 0.5986 0.020 Uiso 1 1 calc R U . . .
C26 C 0.6317(2) 0.51552(19) 0.61397(9) 0.0180(5) Uani 1 1 d . . . . .
H26 H 0.6366 0.5273 0.6515 0.022 Uiso 1 1 calc R U . . .
C27 C 0.7100(3) 0.43164(18) 0.58975(8) 0.0174(4) Uani 1 1 d . . . . .
H27 H 0.7692 0.3862 0.6109 0.021 Uiso 1 1 calc R U . . .
C28 C 0.7021(2) 0.41387(19) 0.53472(8) 0.0144(4) Uani 1 1 d . . . . .
H28 H 0.7558 0.3562 0.5187 0.017 Uiso 1 1 calc R U . . .
C29 C 0.4299(2) 0.44794(18) 0.41127(9) 0.0118(4) Uani 1 1 d . . . . .
C30 C 0.4012(2) 0.4552(2) 0.35646(9) 0.0153(4) Uani 1 1 d . . . . .
H30 H 0.4722 0.4757 0.3321 0.018 Uiso 1 1 calc R U . . .
C31 C 0.2699(2) 0.43247(19) 0.33756(9) 0.0180(5) Uani 1 1 d . . . . .
H31 H 0.2514 0.4362 0.3003 0.022 Uiso 1 1 calc R U . . .
C32 C 0.1650(2) 0.4042(2) 0.37312(9) 0.0171(4) Uani 1 1 d . . . . .
H32 H 0.0747 0.3895 0.3602 0.021 Uiso 1 1 calc R U . . .
C33 C 0.1929(2) 0.39758(19) 0.42764(9) 0.0162(4) Uani 1 1 d . . . . .
H33 H 0.1213 0.3784 0.4520 0.019 Uiso 1 1 calc R U . . .
C34 C 0.3253(2) 0.41901(19) 0.44677(8) 0.0136(4) Uani 1 1 d . . . . .
H34 H 0.3441 0.4138 0.4840 0.016 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C1 1.996(2) . ?
Pd1 O1 2.1082(15) . ?
Pd1 P1 2.2750(6) . ?
Pd1 S1 2.3508(5) . ?
S1 C11 1.786(2) . ?
S1 C8 1.841(2) . ?
P1 C17 1.821(2) . ?
P1 C29 1.822(2) . ?
P1 C23 1.825(2) . ?
O1 C7 1.285(3) . ?
O2 C7 1.232(3) . ?
C1 C6 1.395(3) . ?
C1 C2 1.395(3) . ?
C2 C3 1.397(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.559(3) . ?
C8 C10 1.523(3) . ?
C8 C9 1.539(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.383(3) . ?
C11 C16 1.384(4) . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.364(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.398(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.394(3) . ?
C17 C18 1.399(3) . ?
C18 C19 1.386(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.391(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.383(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.391(3) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.400(3) . ?
C23 C24 1.403(3) . ?
C24 C25 1.391(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.392(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.393(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.391(3) . ?
C29 C30 1.400(3) . ?
C30 C31 1.385(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.391(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.394(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?

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
C1 Pd1 O1 173.34(7) . . ?
C1 Pd1 P1 86.49(6) . . ?
O1 Pd1 P1 100.07(4) . . ?
C1 Pd1 S1 89.36(6) . . ?
O1 Pd1 S1 83.98(4) . . ?
P1 Pd1 S1 170.71(2) . . ?
C11 S1 C8 107.46(11) . . ?
C11 S1 Pd1 96.20(8) . . ?
C8 S1 Pd1 97.63(7) . . ?
C17 P1 C29 101.50(10) . . ?
C17 P1 C23 103.41(10) . . ?
C29 P1 C23 107.29(10) . . ?
C17 P1 Pd1 114.81(7) . . ?
C29 P1 Pd1 109.21(7) . . ?
C23 P1 Pd1 119.00(7) . . ?
C7 O1 Pd1 120.92(14) . . ?
C6 C1 C2 118.8(2) . . ?
C6 C1 Pd1 118.44(16) . . ?
C2 C1 Pd1 122.66(17) . . ?
C1 C2 C3 120.2(2) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.5(2) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 120.8(2) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O2 C7 O1 124.1(2) . . ?
O2 C7 C8 117.6(2) . . ?
O1 C7 C8 118.29(19) . . ?
C10 C8 C9 109.5(2) . . ?
C10 C8 C7 113.42(19) . . ?
C9 C8 C7 107.85(19) . . ?
C10 C8 S1 111.20(17) . . ?
C9 C8 S1 103.18(15) . . ?
C7 C8 S1 111.15(15) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 119.7(2) . . ?
C12 C11 S1 116.47(19) . . ?
C16 C11 S1 123.72(19) . . ?
C11 C12 C13 119.8(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 121.0(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 119.6(3) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C22 C17 C18 119.0(2) . . ?
C22 C17 P1 119.56(17) . . ?
C18 C17 P1 121.45(16) . . ?
C19 C18 C17 120.6(2) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 119.9(2) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 119.9(2) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.4(2) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C17 120.2(2) . . ?
C21 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
C28 C23 C24 118.8(2) . . ?
C28 C23 P1 120.68(16) . . ?
C24 C23 P1 120.48(17) . . ?
C25 C24 C23 120.1(2) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C26 C25 C24 121.0(2) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C25 C26 C27 119.0(2) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
C26 C27 C28 120.5(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C23 120.5(2) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
C34 C29 C30 119.6(2) . . ?
C34 C29 P1 123.77(16) . . ?
C30 C29 P1 116.22(17) . . ?
C31 C30 C29 120.3(2) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 120.1(2) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C33 C32 C31 119.79(19) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 120.28(19) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C29 C34 C33 119.94(19) . . ?
C29 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?

_refine_diff_density_max         0.247
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.048



