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_7047488
_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         '2(C69 H63 N3 P6 Pd4 S3), C H2 Cl2'
_chemical_formula_sum            'C139 H128 Cl2 N6 P12 Pd8 S6'
_chemical_formula_weight         3368.57
_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             2017-02-17
_audit_creation_method
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Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-03-09 deposited with the CCDC.
2018-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.968(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.0071(6)
_cell_length_b                   27.7820(9)
_cell_length_c                   17.5250(6)
_cell_measurement_reflns_used    11585
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.2780
_cell_measurement_theta_min      4.2000
_cell_volume                     7121.5(5)
_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
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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)'
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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -98.00  -48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000 -180.0000 50

  2 omega  -77.00  -51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000   30.0000 26

  3 omega  -48.00  -22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000  -30.0000 26

  4 omega  -84.00  -58.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000 -150.0000 26

  5 omega   51.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -150.0000 25

  6 omega   64.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -30.0000 42

  7 omega    8.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -150.0000 29

  8 omega   36.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -77.0000 -180.0000 29

  9 omega   48.00  103.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  120.0000 55

 10 omega   45.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  120.0000 26

 11 omega   60.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   30.0000 25

 12 omega   16.00   45.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -30.0000 29

 13 omega   10.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  -30.0000 77

 14 omega   13.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   30.0000 26

 15 omega    8.00   38.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  120.0000 30

 16 omega   58.00  110.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000 -120.0000 52

 17 omega   56.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   30.0000 49

 18 omega  -31.00   51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000  -90.0000 82

 19 omega   55.00  114.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 59

 20 omega   42.00  108.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 66

 21 omega   55.00   80.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 25

 22 omega  104.00  145.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 41

 23 omega   59.00  109.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 50

 24 omega  129.00  178.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 49

 25 omega   91.00  167.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -60.0000 76

 26 omega   40.00   85.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 45

 27 omega   38.00   94.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 56

 28 omega   38.00   87.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -150.0000 49

 29 omega   79.00  175.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0638105000
_diffrn_orient_matrix_UB_12      -0.0231853000
_diffrn_orient_matrix_UB_13      -0.0358575000
_diffrn_orient_matrix_UB_21      -0.0385450000
_diffrn_orient_matrix_UB_22      -0.0500221000
_diffrn_orient_matrix_UB_23      0.0057150000
_diffrn_orient_matrix_UB_31      -0.0743283000
_diffrn_orient_matrix_UB_32      0.0060906000
_diffrn_orient_matrix_UB_33      -0.0891044000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         4.390
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22339
_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    1.571
_exptl_crystal_description       plate
_exptl_crystal_F_000             3364
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.122
_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     796
_refine_ls_number_reflns         12702
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+15.5858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9405
_reflns_number_total             12702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02648c3.cif
_cod_data_source_block           20170209
_cod_depositor_comments
'Adding full bibliography for 7047486--7047489.cif.'
_cod_database_code               7047488
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C54H82N2O16P2Pd2
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C70-Cl1
 1.75 with sigma of 0.02
 C70-Cl2
 1.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C70) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C70(0.5) H70A(0.5) H70B(0.5) Cl1(0.5) Cl2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B)
5.b 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), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67), C68(H68)
5.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C64(H64A,H64B,H64C), C69(H69A,H69B,H69C)
;
_olex2_submission_special_instructions 'No special instructions were received'