Synthesis and Characterization of Novel Rhenium(V) Tetradentate N2O2 Schiff Base Monomer and Dimer Complexes
Paul D. Benny; Charles L. Barnes; Pamela M. Piekarski; John D. Lydon; Silvia S. Jurisson; Inorganic Chemistry 42 (2003) 6519–6527; doi:10.1021/ic030240q

data_4314336
_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_contact_author_phone       (573)882-2107
_publ_section_title
;
 Synthesis and Characterization of Novel Rhenium(V) Tetradentate N2O2
 Schiff Base Monomer and Dimer Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6519
_journal_page_last               6527
_journal_paper_doi               10.1021/ic030240q
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C13 H20 Cl N2 O3 Re'
_chemical_formula_weight         473.96
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.1628(5)
_cell_length_b                   13.0699(8)
_cell_length_c                   28.3902(17)
_cell_measurement_reflns_used    6284
_cell_measurement_temperature    173(2)
_cell_volume                     3002.5(3)
_computing_cell_refinement       'SAINT (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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18671
_diffrn_reflns_theta_full        27.16
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    8.280
_exptl_absorpt_correction_T_max  0.32
_exptl_absorpt_correction_T_min  0.21
_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            brown
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.296
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0371P)^2^+6.3044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                4540
_reflns_number_total             6625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030240q_4.cif
_cod_data_source_block           (3)
_cod_database_code               4314336