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_4329493
_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_formula_moiety
'2(C42 H66 Cl3 Mo3 O12 P6 S4), Cl14 Mo6, 3(O)'
_chemical_formula_sum            'C84 H198 Cl20 Mo12 O27 P12 S8'
_chemical_formula_weight         4128.82
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-01-11
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Jan  6 2012 17:48:19, GUI svn.r4021)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   15.3298(3)
_cell_length_b                   15.3298(3)
_cell_length_c                   18.3932(4)
_cell_measurement_reflns_used    7740
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      29.2523
_cell_measurement_theta_min      2.8732
_cell_volume                     3743.35(13)
_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
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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      170.0
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega  -33.00   -1.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  -37.0000    0.0000 32

  2 omega  -84.00   21.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  -26.0000   75.0000 105

  3 omega  -69.00  -43.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596  -37.0000    0.0000 26

  4 omega  -38.00  -13.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596   37.0000   90.0000 25

  5 omega  -38.00   65.00   1.0000  105.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.5596   37.0000 -180.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0069262000
_diffrn_orient_matrix_UB_12      0.0235090000
_diffrn_orient_matrix_UB_13      -0.0343790000
_diffrn_orient_matrix_UB_21      0.0388657000
_diffrn_orient_matrix_UB_22      0.0457656000
_diffrn_orient_matrix_UB_23      0.0147872000
_diffrn_orient_matrix_UB_31      0.0359891000
_diffrn_orient_matrix_UB_32      -0.0143378000
_diffrn_orient_matrix_UB_33      -0.0093314000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28605
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87663
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       plate
_exptl_crystal_F_000             2070
_exptl_crystal_size_max          0.1162
_exptl_crystal_size_mid          0.0952
_exptl_crystal_size_min          0.0248
_refine_diff_density_max         1.555
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         6267
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0608P)^2^+12.1131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                4373
_reflns_number_total             6267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300517g_si_001.cif
_cod_data_source_block           str1249
_cod_database_code               4329493
_chemical_oxdiff_formula         'C42 H96 Cl7 O12 P6 S4 Mo9'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32