Structural and Functional Characteristics of Rhenium Clusters Derived from Redox Chemistry of the Triangular [ReIII3(μ-Cl)3] Core Unit
Daniel Neuman; Patrina Paraskevopoulou; Nikos Psaroudakis; Konstantinos Mertis; Richard J. Staples; Pericles Stavropoulos; Inorganic Chemistry 39 (2000) 5530–5537; doi:10.1021/ic000449t

data_4321598
_publ_section_title
;
 Structural and Functional Characteristics of Rhenium Clusters Derived
 from Redox Chemistry of the Triangular [ReIII3(\m-Cl)3] Core Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5530
_journal_page_last               5537
_journal_paper_doi               10.1021/ic000449t
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety
;
[(C~6~H~5~)~4~P]~2~[Re~3~(\m-Cl)~3~Cl~6.5~(CH~3~CN)1.5(CH~3~C(O)NH)~0.5~] 
;
_chemical_formula_sum            'C52 H46.5 Cl9.5 N2 O0.5 P2 Re3'
_chemical_formula_weight         1664.73
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.719(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1074(2)
_cell_length_b                   23.2153(1)
_cell_length_c                   23.3849(5)
_cell_measurement_reflns_used    93
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      13.67
_cell_measurement_theta_min      2.34
_cell_volume                     5486.75(16)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       '\w, 0.3 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29140
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.162
_exptl_absorpt_correction_T_max  0.914532
_exptl_absorpt_correction_T_min  0.479022
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3172
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.076
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         9642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+35.6822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                8005
_reflns_number_total             9642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000449t_6.cif
_cod_data_source_block           Compound_7
_cod_original_cell_volume        5486.8(2)
_cod_original_formula_sum        'C52 H46.50 Cl9.50 N2 O0.50 P2 Re3'
_cod_database_code               4321598