Diastereoisomeric β-ethyl aspartate‒cobalt(III) complexes: Λ(+)~578~- and Δ({-})~578~-bis(ethane-1,2-diamine)[β-ethyl (<i>S</i>)-aspartato]cobalt(III) bis(perchlorate) monohydrate
Hammershøi, Anders; Schau-Magnussen, Magnus; Bendix, Jesper; Mølgaard, Anne; Acta Crystallographica Section C 66 (2010) m319–m322; doi:10.1107/S0108270110036851

data_2017850
_publ_section_title
;
 Diastereoisomeric \b-ethyl aspartate--cobalt(III) complexes: \L(+)~578~-
 and \D({-})~578~-bis(ethane-1,2-diamine)[\b-ethyl
 (<i>S</i>)-aspartato]cobalt(III) bis(perchlorate) monohydrate
;
_journal_coeditor_code           LG3040
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m319
_journal_page_last               m322
_journal_paper_doi               10.1107/S0108270110036851
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Co (C6 H10 N2 O4) (C2 H8 N2)2] (Cl O4)2 , H2 O'
_chemical_formula_moiety         'C10 H26 Co N5 O4 2+ , 2Cl O4 - , H2 O'
_chemical_formula_sum            'C10 H28 Cl2 Co N5 O13'
_chemical_formula_weight         556.20
_chemical_name_common
;
\D(-)~578~-bis(en)[(S-Asp(OEt)O)]cobalt(III) perchlorate monohydrate
;
_chemical_name_systematic
;
\D(-)~578~-bis(ethane-1,2-diamine)[\b-ethyl (<i>S</i>)-aspartato-
\k^2^<i>N</i>,<i>O</i>^1^]cobalt(III) bis(perchlorate) monohydrate
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.2898(3)
_cell_length_b                   9.2898(3)
_cell_length_c                   48.9696(14)
_cell_measurement_reflns_used    32707
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.66
_cell_volume                     4226.1(2)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f 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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            84126
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Gaussian integration; Coppens, 1970)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.865
_refine_ls_abs_structure_details 'Flack (1983), with 1893 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.017(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4818
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0298P)^2^+3.6785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                4583
_reflns_number_total             4818
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lg3040.cif
_cod_data_source_block           II
_cod_database_code               2017850
_cod_database_fobs_code          2017850