Formation of Group 14 and 15 heteroatom derivatives of trinuclear [M3Se4(H2O)9]4+ (M = Mo, W) and the decreased reactivity of [W3S4(H2O)9]4+
Hernandez-Molina, Rita; Elsegood, Mark R. J.; Clegg, William; Sykes, A. G.; Journal of the Chemical Society, Dalton Transactions  (2001) 2173–; doi:10.1039/b101399h

data_7010633
_publ_section_title
;
 Formation of Group 14 and 15 heteroatom derivatives of trinuclear
 [M3Se4(H2O)9]4+ (M&#x2005;=&#x2005;Mo, W) and the decreased reactivity
 of [W3S4(H2O)9]4+
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2173
_journal_paper_doi               10.1039/b101399h
_journal_year                    2001
_chemical_formula_sum            'C28 H66 Mo3 O31 S4 Se4'
_chemical_formula_weight         1630.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                99.535(2)
_cell_angle_beta                 102.458(2)
_cell_angle_gamma                117.597(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8860(19)
_cell_length_b                   13.8899(19)
_cell_length_c                   17.180(2)
_cell_measurement_reflns_used    4935
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.17
_cell_volume                     2729.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.2116
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17886
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.587
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.137
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     614
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1776
_reflns_number_gt                4724
_reflns_number_total             9356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101399h.txt
_cod_data_source_block           ags36
_cod_original_cell_volume        2729.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010633