Dinuclear Chromium(V) Amino Acid Complexes from the Reduction of Chromium(VI) in the Presence of Amino Acid Ligands: XAFS Characterization of a Chromium(V) Amino Acid Complex
Henrietta A. Headlam; Colin L. Weeks; Peter Turner; Trevor W. Hambley; Peter A. Lay; Inorganic Chemistry 40 (2001) 5097–5105; doi:10.1021/ic010377l

data_4320307
_publ_contact_author_address
;
School of Chemistry
University of Sydney
NSW 2006
Australia
;
_publ_contact_author_email       p.lay@chem.usyd.edu.au
_publ_contact_author_fax         '+61 2 9351 3329'
_publ_contact_author_name        'Peter A. Lay'
_publ_contact_author_phone       '+61 2 9351 4269'
_publ_section_title
;
 Dinuclear Chromium(V) Amino Acid Complexes from the Reduction of
 Chromium(VI) in the Presence of Amino Acid Ligands: XAFS Characterization
 of a Chromium(V) Amino Acid Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5097
_journal_page_last               5105
_journal_paper_doi               10.1021/ic010377l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C12 H24 Cr N3 O6'
_chemical_formula_weight         358.34
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.301(8)
_cell_length_b                   17.301(8)
_cell_length_c                   9.686(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      9.1
_cell_volume                     2511(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_molecular_graphics    'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w:2\q
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1445
_diffrn_reflns_av_sigmaI/netI    0.1733
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            937
_diffrn_reflns_theta_full        59.91
_diffrn_reflns_theta_max         59.91
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        -4.95
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.911
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
analytical (de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1134
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         447
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                221
_reflns_number_total             447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010377l.cif
_cod_data_source_block           pal35
_cod_original_sg_symbol_H-M      'R 3 c '
_cod_database_code               4320307