Synthesis, crystal structure, aqueous speciation, and kinetics of substitution reactions in a water-soluble Mo3S4 cluster bearing hydroxymethyl diphosphine ligands.
Algarra, Andrés G; Basallote, Manuel G.; Fernández-Trujillo, M Jesús; Guillamón, Eva; Llusar, Rosa; Segarra, M. Dolores; Vicent, Cristian; Inorganic chemistry 46 (2007) 7668–7677; doi:10.1021/ic701082p

data_4338878
_publ_section_title
;
 Synthesis, crystal structure, aqueous speciation, and kinetics of
 substitution reactions in a water-soluble Mo3S4 cluster bearing
 hydroxymethyl diphosphine ligands.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7668
_journal_page_last               7677
_journal_paper_doi               10.1021/ic701082p
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C18 H48 Cl4 Mo3 O12 P6 S4'
_chemical_formula_weight         1200.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens
;
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.6863(12)
_cell_length_b                   12.6863(12)
_cell_length_c                   43.813(8)
_cell_measurement_temperature    293(2)
_cell_volume                     6106.7(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16730
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.663
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.080
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0593P)^2^+32.6944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                2924
_reflns_number_total             3983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701082p-file001.cif
_cod_data_source_block           '[Mo3S4Cl3(dhmpe)3]Cl'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        6106.6(14)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4338878
_ratio_of_minimum_to_maximum_apparent_transmission 0.932809