The coordination chemistry of phosphinidene sulfides. Synthesis and catalytic properties of Pd<sub>4</sub> and Pt<sub>4</sub> clusters.
Chai, Jinkui; Tian, Rongqiang; Wu, Di; Wei, Donghui; Xu, Qun; Duan, Zheng; Mathey, François; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13342–13344; doi:10.1039/c8dt02648c

data_7047486
_publ_section_title
;
 The coordination chemistry of phosphinidene sulfides. Synthesis and
 catalytic properties of Pd<sub>4</sub> and Pt<sub>4</sub> clusters.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13342
_journal_page_last               13344
_journal_paper_doi               10.1039/c8dt02648c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C72 H60 P6 Pd4 S3'
_chemical_formula_sum            'C72 H60 P6 Pd4 S3'
_chemical_formula_weight         1632.80
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-16 deposited with the CCDC.
2018-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7902(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.9703(4)
_cell_length_b                   15.48579(16)
_cell_length_c                   29.9766(4)
_cell_measurement_reflns_used    21516
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5280
_cell_measurement_theta_min      3.5470
_cell_volume                     15271.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -75.00  -49.80   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9984  126.0000  143.0000 63

  2 omega  -86.00  -60.80   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9984  144.0000  -48.0000 63

  3 omega    3.00   28.20   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546 -126.0000   66.0000 63

  4 omega   15.00   94.20   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546 -144.0000 -101.0000 198

  5 omega -104.00  -74.80   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -20.9984  178.0000 -150.0000 73

  6 omega   60.00   94.00   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546   57.0000   60.0000 85

  7 omega   37.00   92.20   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546   57.0000 -180.0000 138

  8 omega  -46.00   48.00   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546  -57.0000   30.0000 235

  9 omega    2.00   28.00   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546   57.0000   60.0000 65

 10 omega   38.00   65.20   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546  178.0000 -150.0000 68

 11 omega   55.80  105.00   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546  178.0000 -120.0000 123

 12 omega   -9.00   98.20   0.4000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       23.6546   37.0000  -30.0000 268
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0203541000
_diffrn_orient_matrix_UB_12      -0.0010147000
_diffrn_orient_matrix_UB_13      0.0062960000
_diffrn_orient_matrix_UB_21      -0.0070092000
_diffrn_orient_matrix_UB_22      -0.0041750000
_diffrn_orient_matrix_UB_23      -0.0227840000
_diffrn_orient_matrix_UB_31      0.0011026000
_diffrn_orient_matrix_UB_32      -0.0455940000
_diffrn_orient_matrix_UB_33      0.0019484000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            72563
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.779
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       prism
_exptl_crystal_F_000             6512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         15589
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0500P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12445
_reflns_number_total             15589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02648c3.cif
_cod_data_source_block           201610168b
_cod_depositor_comments
'Adding full bibliography for 7047486--7047489.cif.'
_cod_database_code               7047486
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C37H42N1O3S1P2Pd1
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C56, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C57) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(C56) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_olex2_submission_special_instructions 'No special instructions were received'