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_7047489
_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         'C66 H54 P6 Pd4 S6'
_chemical_formula_sum            'C66 H54 P6 Pd4 S6'
_chemical_formula_weight         1650.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.931(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6070(3)
_cell_length_b                   27.8868(3)
_cell_length_c                   17.6155(3)
_cell_measurement_reflns_used    12596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1560
_cell_measurement_theta_min      3.5850
_cell_volume                     7060.9(2)
_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  -32.00   -2.90   0.3000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.1755   37.0000  -90.0000 97

  2 omega  -21.00   23.10   0.3000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.1755  -99.0000  -90.0000 147

  3 omega    6.00   85.20   0.3000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   37.0000 -150.0000 264

  4 omega  -23.00   55.00   0.3000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -99.0000   90.0000 260

  5 omega   35.00   71.00   0.3000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  178.0000 -120.0000 120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0297606000
_diffrn_orient_matrix_UB_12      0.0125284000
_diffrn_orient_matrix_UB_13      -0.0149982000
_diffrn_orient_matrix_UB_21      0.0212961000
_diffrn_orient_matrix_UB_22      -0.0219528000
_diffrn_orient_matrix_UB_23      -0.0032073000
_diffrn_orient_matrix_UB_31      -0.0331056000
_diffrn_orient_matrix_UB_32      -0.0028562000
_diffrn_orient_matrix_UB_33      -0.0409387000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37057
_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         26.371
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91428
_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    1.553
_exptl_crystal_description       prism
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.268
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         14396
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0371
_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/[\s^2^(Fo^2^)+(0.0387P)^2^+3.5160P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11547
_reflns_number_total             14396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02648c3.cif
_cod_data_source_block           201610169
_cod_depositor_comments
'Adding full bibliography for 7047486--7047489.cif.'
_cod_database_code               7047489
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C37H42N1O3S1P2Pd1
_reflns_odcompleteness_completeness 99.67
_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
2. Restrained distances
 C1-C2A
 1.4 with sigma of 0.02
 C2A-C4
 1.4 with sigma of 0.02
 C7-C8
 1.4 with sigma of 0.02
 C6-C5
 1.4 with sigma of 0.02
 C6A-C5
 1.4 with sigma of 0.02
 C6A-C8
 1.4 with sigma of 0.02
 C7-C6
 1.4 with sigma of 0.02
 C8-C6
 2.2 with sigma of 0.02
 C6-C7
 1.4 with sigma of 0.02
3. Restrained planarity
 C1, C2A, C3, C4, S4A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C65) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(S6) = Uanis(S6A)
Uanis(C10) = Uanis(C10A)
Uanis(S4) = Uanis(S4A)
Uanis(C2) = Uanis(C2A)
Uanis(S5) = Uanis(S5A)
Uanis(C6) = Uanis(C6A)
5. Others
 Sof(C10A)=Sof(H10A)=Sof(H11A)=Sof(H12A)=Sof(S6A)=1-FVAR(1)
 Sof(C10)=Sof(H10)=Sof(H11)=Sof(H12)=Sof(S6)=FVAR(1)
 Sof(C2A)=Sof(H2A)=Sof(H3B)=Sof(H4B)=Sof(S4A)=1-FVAR(2)
 Sof(C2)=Sof(H2)=Sof(H3A)=Sof(H4A)=Sof(S4)=FVAR(2)
 Sof(C6A)=Sof(H6A)=Sof(H7B)=Sof(H8B)=Sof(S5A)=1-FVAR(3)
 Sof(C6)=Sof(H6)=Sof(H7A)=Sof(H8A)=Sof(S5)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A), C3(H3A), C3(H3B), C4(H4B), C4(H4A), C6(H6), C6A(H6A),
 C7(H7A), C7(H7B), C8(H8B), C8(H8A), C10(H10), C10A(H10A), C11(H11), C11(H11A),
 C12(H12A), 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)
;
_olex2_submission_special_instructions 'No special instructions were received'