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_4308996
_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            'C48 H48 F6 N2 O2.5 P3 Re'
_chemical_formula_weight         1085.99
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                95.5220(10)
_cell_angle_beta                 97.1300(10)
_cell_angle_gamma                91.3500(10)
_cell_formula_units_Z            4
_cell_length_a                   18.8261(12)
_cell_length_b                   16.2517(10)
_cell_length_c                   15.4556(10)
_cell_measurement_reflns_used    8348
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.2
_cell_volume                     4667.4(5)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33573
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    2.772
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.40
_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            red
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         20133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                15894
_reflns_number_total             20133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048670jsi20041005_112717_2.cif
_cod_data_source_block           (1)
_cod_original_formula_sum        'C48 H48 F6 N2 O2.50 P3 Re'
_cod_database_code               4308996