Investigation of Mixed Oxidation State Cyanide-Bridged ReVOxo (acac2en/pn) and ReI(bipy)(CO)3 Complexes
Adam L. Moore; Brendan Twamley; Charles L. Barnes; Paul D. Benny; Inorganic Chemistry 50 (2011) 4686–4688; doi:10.1021/ic2005002

data_4325284
_publ_contact_author_address
;Department of Chemistry, 
Washington State University, 
PO Box 644630, 
Pullman, 
WA 99164, 
USA
;
_publ_contact_author_email       bennyp@wsu.edu
_publ_contact_author_name        'Paul D. Benny'
_publ_section_title
;
 Investigation of Mixed Oxidation State Cyanide-Bridged ReVOxo
 (acac2en/pn) and ReI(bipy)(CO)3 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4686
_journal_page_last               4688
_journal_paper_doi               10.1021/ic2005002
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C27 H28 N5 O6 Re2, F6 P'
_chemical_formula_sum            'C27 H28 F6 N5 O6 P Re2'
_chemical_formula_weight         1035.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 100.845(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1658(6)
_cell_length_b                   12.5539(4)
_cell_length_c                   15.1201(5)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     3200.15(19)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28777
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    7.692
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.468
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0449P)^2^+1.1487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                6595
_reflns_number_total             7385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2005002_si_002_1.cif
_cod_data_source_block           cmpd4
_cod_original_cell_volume        3200.15(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4325284