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_7004434
_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
'2 C36 H88 N3 P6 Re6 Se8 3+, 3 Sb F6 -, 3 Br -, H Br'
_chemical_formula_sum            'C72 H177 Br4 F18 N6 P12 Re12 Sb3 Se16'
_chemical_formula_weight         6023.49
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.451(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.752(5)
_cell_length_b                   28.000(3)
_cell_length_c                   24.028(3)
_cell_measurement_reflns_used    5938
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.15
_cell_volume                     30812(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND 3 (Brandenburg & Putz, 2004)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81358
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.897
_exptl_absorpt_correction_T_max  0.2119
_exptl_absorpt_correction_T_min  0.0636
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2007'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    2.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             21840
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.392
_refine_diff_density_min         -3.429
_refine_diff_density_rms         0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1304
_refine_ls_number_reflns         19916
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0565P)^2^+5373.5254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                11506
_reflns_number_total             19916
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            B806888G.txt
_cod_data_source_block           zz135
_cod_original_cell_volume        30811(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7004434