Unusual Reactivity of the {ReVO}3+ Core: Syntheses and Characterization of Novel Rhenium Halide Complexes with N-Methyl-o-diaminobenzene
Lihui Wei; John W. Babich; Jon Zubieta; Inorganic Chemistry 43 (2004) 6445–6454; doi:10.1021/ic049372p

data_4311676
_publ_contact_author_address
;Department of Chemistry
1-014 CST
Syracuse University
111 College Place
Syracuse, NY 13244
;
_publ_contact_author_email       jazubiet@syr.edu
_publ_contact_author_fax         315-443-4070
_publ_contact_author_name        'Jon Zubieta'
_publ_contact_author_phone       315-443-2547
_publ_section_title
;
 Unusual Reactivity of the {ReVO}3+ Core: Syntheses and Characterization
 of Novel Rhenium Halide Complexes with N-Methyl-o-diaminobenzene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6445
_journal_page_last               6454
_journal_paper_doi               10.1021/ic049372p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C18 H15 Cl2 O P Re0.5'
_chemical_formula_weight         442.27
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.0950(10)
_cell_angle_beta                 108.2160(10)
_cell_angle_gamma                93.8760(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2986(6)
_cell_length_b                   9.6486(6)
_cell_length_c                   10.3467(7)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.14
_cell_volume                     853.30(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Platfrom w/APEX CCD detector'
_diffrn_measurement_method       'Phi and omega scan'
_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    0.0938
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11237
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    4.000
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_correction_T_min  0.7953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 97)'
_exptl_crystal_colour            res
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             435
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.250
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                4843
_reflns_number_total             5579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049372psi20040712_033522.cif
_cod_data_source_block           p-1
_cod_original_formula_sum        'C18 H15 Cl2 O P Re0.50'
_cod_database_code               4311676