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_4341322
_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 Cr2 O7 P3'
_chemical_formula_sum            'C7 H7 Cr2 O7 P3'
_chemical_formula_weight         400.04
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-07-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                111.796(12)
_cell_angle_beta                 92.150(10)
_cell_angle_gamma                115.204(14)
_cell_formula_units_Z            1
_cell_length_a                   6.9134(9)
_cell_length_b                   7.3239(10)
_cell_length_c                   8.7610(10)
_cell_measurement_reflns_used    2151
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      66.4330
_cell_measurement_theta_min      5.5550
_cell_volume                     362.43(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5431
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega   29.60  116.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   37.0000  -30.0000 54

  2 omega   12.00  109.60   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000 -150.0000 61

  3 omega    8.00   89.60   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306 -125.0000  120.0000 51

  4 omega -121.00  -93.80   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  125.0000    0.0000 17

  5 omega   15.00  109.40   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  -30.0000 59

  6 omega   29.00   73.80   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 28

  7 omega   94.00  126.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -86.0000  163.0000 20

  8 omega   63.00  160.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   30.0000 61

  9 omega   19.00   65.40   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 29

 10 omega   40.00  161.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000 -180.0000 76

 11 omega   17.00   68.20   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -86.0000  163.0000 32

 12 omega   10.00  131.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000   94.0000 76

 13 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000  150.0000 70

 14 omega  -37.00   63.80   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306  -37.0000  150.0000 63

 15 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000   60.0000 70

 16 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 70

 17 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -30.0000 70

 18 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   90.0000 70

 19 omega   19.00   75.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 35

 20 omega   60.00  172.00   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -60.0000 70

 21 omega   66.00  165.20   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -90.0000 62

 22 omega  -97.00  -20.20   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6306  125.0000  -60.0000 48

 23 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000    0.0000 70

 24 omega    6.00  118.00   1.6000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6306   77.0000  -60.0000 70

 25 omega   15.00   80.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000 -105.0000 41

 26 omega   60.00  117.60   1.6000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -150.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1375204000
_diffrn_orient_matrix_UB_12      0.1208994000
_diffrn_orient_matrix_UB_13      -0.0998276000
_diffrn_orient_matrix_UB_21      0.1121110000
_diffrn_orient_matrix_UB_22      0.2197174000
_diffrn_orient_matrix_UB_23      0.1626865000
_diffrn_orient_matrix_UB_31      0.1807011000
_diffrn_orient_matrix_UB_32      -0.0574347000
_diffrn_orient_matrix_UB_33      0.0385881000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4479
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.631
_diffrn_reflns_theta_min         5.592
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.728
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.014
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       plate
_exptl_crystal_F_000             198
_exptl_crystal_recrystallization_method
'The material was recrystallised from THF by cooling to -25'
_exptl_crystal_size_max          0.5603
_exptl_crystal_size_mid          0.1536
_exptl_crystal_size_min          0.0097
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1250
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0654P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1097
_reflns_number_total             1250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5012082_si_005.cif
_cod_data_source_block           neu
_cod_depositor_comments
'Adding full bibliography for 4341321--4341322.cif.'
_cod_original_cell_volume        362.42(9)
_cod_database_code               4341322
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C7 H7 O7 P3 W2'
_reflns_odcompleteness_completeness 96.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All P(H,H) groups
 At 1.5 times of:
  All P(H,H,H) groups
2. Restrained distances
 P2-H2A = P2-H2B = P2-H2C = P3-H3A = P3-H3C = P3-H3B
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P2 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: P2(0.32) H2A(0.32) H2B(0.32) H2C(0.32) C4(0.82) O4(0.82) O2(0.68)
 C2(0.68) P3(0.18) H3A(0.18) H3B(0.18) H3C(0.18)
5.a Secondary CH2 refined with riding coordinates and stretchable bonds:
 P1(H1A,H1B)
5.b Idealised Me refined with riding coordinates and stretchable bonds:
 P2(H2A,H2B,H2C), P3(H3A,H3B,H3C)
;
_shelx_res_checksum              42667
_shelx_hkl_checksum              51978
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with inert oil'
_olex2_submission_special_instructions 'No special instructions were received'