Redetermination of bis(acetonitrile-κ<i>N</i>)octa-μ~3~-selenido-tetrakis(triethylphosphine-κ<i>P</i>)hexarhenium(III) at 150K
Orto, Peter J; Nichol, Gary S; Zheng, Zhiping; Acta Crystallographica Section E 63 (2007) m678–m679; doi:10.1107/S1600536807004989

data_2212634
_publ_section_title
;Redetermination of
 bis(acetonitrile-\k<i>N</i>)octa-\m~3~-selenido-tetrakis(triethylphosphine-\k<i>P</i>)hexarhenium(III)
 at 150K
;
_journal_coeditor_code           LH2304
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m678
_journal_page_last               m679
_journal_paper_doi               10.1107/S1600536807004989
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Re6 Se8 (C2 H3 N1)2 (C6 H15 P1)4] (Sb F6)2'
_chemical_formula_moiety         'C28 H66 N2 P4 Re6 Se8 2+ , 2 Sb F6 -'
_chemical_formula_sum            'C28 H66 F12 N2 P4 Re6 Sb2 Se8'
_chemical_formula_weight         2775.09
_chemical_name_systematic
;
bis(acetonitrile-\kN)octa-\m~3~selenido-tetrakis(triethylphosphine-
\kP)hexarhenium(III)
;
_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   difmap
_atom_sites_solution_primary     'using known coordinates'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.010(3)
_cell_length_b                   17.155(3)
_cell_length_c                   13.438(3)
_cell_measurement_reflns_used    17172
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     2893.7(11)
_computing_cell_refinement       'EvalCCD (Duisenberg <i>et al.</i>,  2003)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'using known coordinates (Reference?)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30352
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.618
_exptl_absorpt_correction_T_max  0.0502
_exptl_absorpt_correction_T_min  0.0305
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.796
_refine_diff_density_min         -1.006
_refine_ls_extinction_coef       0.000341(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2001)'
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+7.3346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                5470
_reflns_number_total             6605
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2304.cif
_cod_data_source_block           I
_cod_original_cell_volume        2893.8(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2212634
_cod_database_fobs_code          2212634