Transition-metal complexes containing parent phosphine or phosphinyl ligands and their use as precursors for phosphide nanoparticles.
Bauer, Susanne; Hunger, Cornelia; Bodensteiner, Michael; Ojo, Wilfried-Solo; Cros-Gagneux, Arnaud; Chaudret, Bruno; Nayral, Céline; Delpech, Fabien; Scheer, Manfred; Inorganic chemistry 53 (2014) 11438–11446; doi:10.1021/ic5012082

data_4341321
_publ_section_title
;
 Transition-metal complexes containing parent phosphine or phosphinyl
 ligands and their use as precursors for phosphide nanoparticles.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11438
_journal_page_last               11446
_journal_paper_doi               10.1021/ic5012082
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C7 H7 O7 P3 W2'
_chemical_formula_sum            'C7 H7 O7 P3 W2'
_chemical_formula_weight         663.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-08-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
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_cell_length_b                   7.4298(10)
_cell_length_c                   8.8711(13)
_cell_measurement_reflns_used    4082
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      66.6586
_cell_measurement_theta_min      5.4898
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_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
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;
  1 omega  -99.00  -53.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6137  179.0000 -120.0000 23

  2 omega    7.00   41.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6137  -77.0000 -120.0000 17

  3 omega   34.00   62.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6137  179.0000  150.0000 14

  4 omega  -36.00    6.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6137  -77.0000 -120.0000 21

  5 omega  -66.00  -38.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6137  -77.0000 -120.0000 14

  6 omega   62.00  100.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6137  179.0000  150.0000 19

  7 omega   -6.00   24.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega  -35.00   27.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   26.00   58.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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 10 omega   -3.00   25.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   84.0000    3.0000 14

 11 omega   21.00   53.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   77.0000  165.0000 16

 12 omega   10.00   38.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   79.0000   93.0000 14

 13 omega  -73.00  -27.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -52.0000  -75.0000 -176.0000 23

 14 omega -129.00  -83.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -52.0000  -75.0000 -176.0000 23

 15 omega  -66.00  -22.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -56.0000  -79.0000 -133.0000 22

 16 omega  -46.00  -20.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
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 17 omega   24.00   60.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   14.0000 18

 18 omega  -66.00  -28.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -62.0000  -77.0000  -62.0000 19

 19 omega  -56.00  -28.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -62.0000  -79.0000    1.0000 14

 20 omega   33.00   63.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000   95.0000 15

 21 omega  -73.00  -43.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.0000  -75.0000 -157.0000 15

 22 omega  -68.00  -40.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -72.0000  -71.0000  -13.0000 14

 23 omega  -76.00  -40.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -72.0000  -69.0000  131.0000 18

 24 omega  -69.00  -41.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -74.0000  -71.0000  -41.0000 14

 25 omega  -72.00  -42.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -74.0000  -71.0000   88.0000 15

 26 omega  -80.00  -42.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -76.0000  -73.0000 -112.0000 19

 27 omega  -73.00  -45.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -78.0000  -77.0000   71.0000 14

 28 omega  -82.00  -48.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -80.0000  -68.0000 -135.0000 17

 29 omega  -80.00  -50.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -80.0000  -68.0000   15.0000 15

 30 omega  -84.00  -48.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -82.0000  -77.0000  -69.0000 18

 31 omega -111.00  -19.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  125.0000  -90.0000 46

 32 omega  -87.00  -57.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -77.0000 -150.0000 15

 33 omega  -96.00  -58.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -71.0000   73.0000 19

 34 omega -164.00 -104.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -71.0000   73.0000 30

 35 omega -112.00  -70.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  125.0000    0.0000 21

 36 omega  -88.00  -58.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -69.0000   -6.0000 15

 37 omega -144.00  -98.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -69.0000   -6.0000 23

 38 omega -153.00  -61.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -63.0000  107.0000 46

 39 omega -118.00  -88.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -75.0000   34.0000 15

 40 omega -156.00 -126.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -75.0000   34.0000 15

 41 omega  -92.00  -56.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -77.0000  150.0000 18

 42 omega -145.00  -59.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -65.0000  -70.0000 43

 43 omega -166.00 -122.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -77.0000  150.0000 22

 44 omega  -87.00  -57.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  -77.0000  -30.0000 15

 45 omega   15.00   65.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000   30.0000 25

 46 omega  125.00  151.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   60.0000 13

 47 omega   60.00   96.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   60.0000 18

 48 omega   61.00  133.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000    0.0000 36

 49 omega  108.00  172.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -90.0000 32

 50 omega   74.00  102.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -90.0000 14

 51 omega  136.00  164.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -120.0000 14

 52 omega   66.00  112.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -120.0000 23

 53 omega   98.00  156.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 29

 54 omega   63.00  127.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  120.0000 32

 55 omega   61.00   91.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 15

 56 omega   65.00  127.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  120.0000 31

 57 omega   62.00  172.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -150.0000 55

 58 omega  134.00  164.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  120.0000 15

 59 omega   77.00  129.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  120.0000 26

 60 omega   78.00  120.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -48.0000  152.0000 21

 61 omega   27.00   59.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -48.0000  152.0000 16

 62 omega   68.00  128.00   2.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000   30.0000 30
;
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Ruby (Gemini ultra Cu)'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_12      0.0043586325
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_diffrn_orient_matrix_UB_32      -0.0086478293
_diffrn_orient_matrix_UB_33      0.1532137982
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
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_diffrn_reflns_av_unetI/netI     0.0887
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_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.530
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_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.876
_exptl_crystal_description       rod
_exptl_crystal_F_000             298
_exptl_crystal_size_max          0.1173
_exptl_crystal_size_mid          0.0663
_exptl_crystal_size_min          0.0281
_refine_diff_density_max         3.077
_refine_diff_density_min         -3.033
_refine_diff_density_rms         0.431
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1312
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+2.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1224
_reflns_number_total             1312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5012082_si_006.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4341321--4341322.cif.'
_cod_original_cell_volume        383.24(11)
_cod_database_code               4341321
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'W2 P3 C7 O7 H7'
_olex2_refinement_description
;
1. Others
 Fixed Sof: C2(0.86) O2(0.86) P2(0.36) H2A(0.36) H2B(0.36) H2C(0.36) C4(0.64)
 O4(0.64) P3(0.14) H3A(0.14) H3B(0.14) H3C(0.14)
 Fixed Uiso: H2A(0.053) H2B(0.053) H2C(0.053) H1A(0.028) H1B(0.028) H3A(0.056)
 H3B(0.056) H3C(0.056)
;
_shelx_res_checksum              67043
_shelx_hkl_checksum              29739
_olex2_submission_original_sample_id 3b_neu
_olex2_submission_special_instructions 'No special instructions were received'