Complexes of the [Re6(μ3-Se)8]2+ core-containing clusters with the water-soluble 1,3,5-triaza-7-phosphaadamantane (PTA) ligand: unexpected ligand protonation and related studies
Tu, Xiaoyan; Nichol, Gary S.; Wang, Ruiyao; Zheng, Zhiping; Dalton Transactions  (2008) 6030–6038; doi:10.1039/B806888G

data_7004433
_publ_section_title
;
 Complexes of the [Re6(\m3-Se)8]2+ core-containing clusters with the
 water-soluble 1,3,5-triaza-7-phosphaadamantane (PTA) ligand:
 unexpected ligand protonation and related studies
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              6030
_journal_page_last               6038
_journal_paper_doi               10.1039/B806888G
_journal_year                    2008
_chemical_formula_moiety
'C36 H87 N3 P6 Re6 Se8 2+, C36 H88 N3 P6 Re6 Se8 3+, 5 Sb F6 -'
_chemical_formula_sum            'C72 H175 F30 N6 P12 Re12 Sb5 Se16'
_chemical_formula_weight         6173.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.71(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.183(5)
_cell_length_b                   23.994(5)
_cell_length_c                   24.244(5)
_cell_measurement_reflns_used    248413
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.5
_cell_volume                     14290(5)
_computing_cell_refinement       'EvalCCD (Duisenberg et al. 2003)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg & Putz, 2004)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            116611
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.327
_exptl_absorpt_correction_T_max  0.5145
_exptl_absorpt_correction_T_min  0.0741
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2007'
_exptl_crystal_colour            orangel
_exptl_crystal_density_diffrn    2.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             11192
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.436
_refine_diff_density_min         -2.227
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1433
_refine_ls_number_reflns         18553
_refine_ls_number_restraints     401
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+1103.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                12250
_reflns_number_total             18553
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            B806888G.txt
_cod_data_source_block           zz134
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7004433