μ-Hydroxido-bis[(2,2'-bipyridine)tricarbonylrhenium(I)] perrhenate
Ruth, Kai; Morawitz, Thorsten; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 64 (2008) m496–; doi:10.1107/S160053680800490X

data_2217713
_publ_section_title
;
 \m-Hydroxido-bis[(2,2'-bipyridine)tricarbonylrhenium(I)] perrhenate
;
_journal_coeditor_code           AT2546
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m496
_journal_paper_doi               10.1107/S160053680800490X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Re2 (O H) (C10 H8 N2)2 (C O)6] [Re O4]'
_chemical_formula_moiety         'C26 H17 N4 O7 Re2 +, O4 Re -'
_chemical_formula_sum            'C26 H17 N4 O11 Re3'
_chemical_formula_weight         1120.04
_chemical_name_systematic
;
\m-Hydroxido-bis[(2,2'-bipyridine)tricarbonylrhenium(I)] perrhenate
;
_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                96.488(7)
_cell_angle_beta                 94.768(7)
_cell_angle_gamma                104.038(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0304(7)
_cell_length_b                   11.0506(9)
_cell_length_c                   15.5152(13)
_cell_measurement_reflns_used    19460
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      3.8
_cell_volume                     1482.6(2)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe IPDSII two-circle'
_diffrn_measurement_method       \w
_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  0.0896
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21159
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         3.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.282
_exptl_absorpt_correction_T_max  0.1882
_exptl_absorpt_correction_T_min  0.1425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.565
_refine_diff_density_min         -5.650
_refine_ls_extinction_coef       0.0058(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1565P)^2^+50.8834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2618
_reflns_number_gt                4782
_reflns_number_total             5550
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2546.cif
_cod_data_source_block           I
_cod_database_code               2217713
_cod_database_fobs_code          2217713