Water-Soluble Mo3S4 Clusters Bearing Hydroxypropyl Diphosphine Ligands: Synthesis, Crystal Structure, Aqueous Speciation, and Kinetics of Substitution Reactions
Manuel G. Basallote; M. Jesús Fernández-Trujillo; Jose Ángel Pino-Chamorro; Tomás F. Beltrán; Carolina Corao; Rosa Llusar; Maxim Sokolov; Cristian Vicent; Inorganic Chemistry 51 (2012) 6794–6802; doi:10.1021/ic300517g

data_4329494
_publ_contact_author_name
;
;
_publ_section_title
;
 Water-Soluble Mo3S4 Clusters Bearing Hydroxypropyl Diphosphine Ligands:
 Synthesis, Crystal Structure, Aqueous Speciation, and Kinetics of
 Substitution Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6794
_journal_page_last               6802
_journal_paper_doi               10.1021/ic300517g
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H79 Mo3 O12 P6 S4, F6 P, 5(O)'
_chemical_formula_sum            'C42 H133 F6 Mo3 O17 P7 S4'
_chemical_formula_weight         1657.33
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-05-15
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.184(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.4129(10)
_cell_length_b                   15.3050(5)
_cell_length_c                   18.5707(7)
_cell_measurement_reflns_used    13120
_cell_measurement_temperature    167.7
_cell_measurement_theta_max      29.3063
_cell_measurement_theta_min      2.8956
_cell_volume                     7132.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      167.7
_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  -60.00  -31.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  136.0000   76.0000 29

  2 omega  -30.00   54.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596   37.0000  -30.0000 84

  3 omega  -45.00  -18.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627  -77.0000 -120.0000 27

  4 omega  -14.00   13.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627  -37.0000  120.0000 27

  5 omega  -57.00  -30.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627  -37.0000  -30.0000 27

  6 omega  -20.00   91.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627   77.0000   60.0000 111

  7 omega  -86.00  -45.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  151.0000  121.0000 41

  8 omega  -14.00   88.00   1.0000   34.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2627   37.0000  -30.0000 102
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0081367000
_diffrn_orient_matrix_UB_12      -0.0399801000
_diffrn_orient_matrix_UB_13      0.0122457000
_diffrn_orient_matrix_UB_21      0.0121558000
_diffrn_orient_matrix_UB_22      -0.0233938000
_diffrn_orient_matrix_UB_23      -0.0231943000
_diffrn_orient_matrix_UB_31      0.0241890000
_diffrn_orient_matrix_UB_32      -0.0016566000
_diffrn_orient_matrix_UB_33      0.0304686000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35148
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brownish
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         11948
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+14.7125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                10375
_reflns_number_total             11948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300517g_si_002.cif
_cod_data_source_block           str1250
_cod_original_cell_volume        7132.3(4)
_cod_database_code               4329494
_chemical_oxdiff_formula         'C42 H133 F6 Mo3 O17 P7 S4'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32