Reactivity of Rhenium(V) Oxo Schiff Base Complexes with Phosphine Ligands: Rearrangement and Reduction Reactions
Paul D. Benny; Jenny L. Green; Hendrik P. Engelbrecht; Charles L. Barnes; Silvia S. Jurisson; Inorganic Chemistry 44 (2005) 2381–2390; doi:10.1021/ic048670j

data_4308998
_publ_contact_author
;
Dr. Silvia Jurisson
Department of Chemistry
University of Missouri - Columbia
Columbia, Missouri 65211 USA
;
_publ_contact_author_email       JurissonS@missouri.edu
_publ_contact_author_fax         (573)882-2754
_publ_section_title
;
Reactivity of Rhenium(V) Oxo Schiff Base Complexes with Phosphine
Ligands: Rearrangement and Reduction Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2381
_journal_page_last               2390
_journal_paper_doi               10.1021/ic048670j
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C18 H33 F7.5 N2 O3 P2.25 Re'
_chemical_formula_weight         723.85
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.7730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   39.8194(15)
_cell_length_b                   13.6187(5)
_cell_length_c                   20.1777(8)
_cell_measurement_reflns_used    8561
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.2
_cell_volume                     10419.9(7)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_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 SMART CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31795
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.07
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    4.879
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.31
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Data were corrected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5684
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.874
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0505P)^2^+8.0192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                7086
_reflns_number_total             11497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048670jsi20041005_112717_4.cif
_cod_data_source_block           (3)
_cod_original_formula_sum        'C18 H33 F7.50 N2 O3 P2.25 Re'
_cod_database_code               4308998