Influence of the Ligand Alkyl Chain Length on the Solubility, Aqueous Speciation, and Kinetics of Substitution Reactions of Water-Soluble M3S4 (M = Mo, W) Clusters Bearing Hydroxyalkyl Diphosphines
Tomás F. Beltrán; Rosa Llusar; Maxim Sokolov; Manuel G. Basallote; M. Jesús Fernández-Trujillo; Jose Ángel Pino-Chamorro; Inorganic Chemistry 52 (2013) 8713–8722; doi:10.1021/ic400897y

data_4335555
_publ_contact_author_name
;
;
_publ_section_title
;
 Influence of the Ligand Alkyl Chain Length on the Solubility, Aqueous
 Speciation, and Kinetics of Substitution Reactions of Water-Soluble M3S4
 (M = Mo, W) Clusters Bearing Hydroxyalkyl Diphosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8713
_journal_page_last               8722
_journal_paper_doi               10.1021/ic400897y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'C54 H82 Cl3 Mo3 O12 P6 S4, 1.5(Cl14 Mo6), 2(O)'
_chemical_formula_sum            'C54 H121.99 Cl24 Mo12 O14 P6 S4'
_chemical_formula_weight         3311.65
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-18
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                105.456(3)
_cell_angle_beta                 103.923(2)
_cell_angle_gamma                105.522(3)
_cell_formula_units_Z            2
_cell_length_a                   14.5081(4)
_cell_length_b                   20.1247(7)
_cell_length_c                   25.1681(6)
_cell_measurement_reflns_used    22047
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      29.2937
_cell_measurement_theta_min      2.8134
_cell_volume                     6427.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -14.00   62.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596   57.0000 -120.0000 76

  2 omega  -66.00    9.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  -57.0000  150.0000 75

  3 omega  -99.00  -74.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  178.0000  -30.0000 25

  4 omega  -19.00   30.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  -99.0000   30.0000 49

  5 omega  -83.00  -32.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  -37.0000  -90.0000 51

  6 omega  -99.00  -55.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  178.0000 -150.0000 44

  7 omega  -81.00  -56.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  178.0000  150.0000 25

  8 omega  -16.00    9.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  -99.0000 -150.0000 25

  9 omega  -56.00   14.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596   19.0000 -150.0000 70

 10 omega    2.00   28.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627  -57.0000  -30.0000 26

 11 omega   34.00   74.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627 -178.0000  120.0000 40

 12 omega  -52.00   -9.00   1.0000   27.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627  -57.0000  -90.0000 43
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0035244000
_diffrn_orient_matrix_UB_12      -0.0372340000
_diffrn_orient_matrix_UB_13      -0.0057709000
_diffrn_orient_matrix_UB_21      0.0243891000
_diffrn_orient_matrix_UB_22      0.0021246000
_diffrn_orient_matrix_UB_23      -0.0210884000
_diffrn_orient_matrix_UB_31      0.0479038000
_diffrn_orient_matrix_UB_32      0.0117743000
_diffrn_orient_matrix_UB_33      0.0220380000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            81900
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.805
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'greenish green'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.3012
_exptl_crystal_size_mid          0.0694
_exptl_crystal_size_min          0.0474
_refine_diff_density_max         2.854
_refine_diff_density_min         -2.284
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         25222
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+57.6264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2375
_reflns_number_gt                17178
_reflns_number_total             25222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400897y_si_002.cif
_cod_data_source_block           str1254
_cod_original_cell_volume        6427.8(3)
_cod_database_code               4335555
_chemical_oxdiff_formula         'C54 H120 Cl17 P6 S4 O12 Mo9'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32