Metal complex amino acid synthons: syntheses, structures and stereoselective reactions of (iminoacetato)cobalt(iii) complexes
Bendahl, Lars; Hammershøi, Anders; Jensen, Dan Kjærgaard; Larsen, Sine; Riisager, Anders; Sargeson, Alan M.; Sørensen, Henning Osholm; Journal of the Chemical Society, Dalton Transactions  (2002) 3054–; doi:10.1039/b202090d

data_7011599
_publ_section_title
;
 Metal complex amino acid synthons: syntheses, structures and
 stereoselective reactions of (iminoacetato)cobalt(iii) complexes
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3054
_journal_paper_doi               10.1039/b202090d
_journal_year                    2002
_chemical_formula_moiety         'C7 H20 Co N5, S2 O6 , 1.5 H2 O'
_chemical_formula_sum            'C7 H23 Co N5 O9.5 S2'
_chemical_formula_weight         452.35
_chemical_name_systematic
; 
[(en)2Co(O2CCH=NMe)]S2O6,1.5H2O 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and manual editing'
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.7780(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.3390(2)
_cell_length_b                   16.3540(3)
_cell_length_c                   14.3640(3)
_cell_measurement_reflns_used    179
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      3.1
_cell_volume                     1721.97(7)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'Ortep II (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\q 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57596
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.295
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         7557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+2.1714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                6691
_reflns_number_total             7557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202090d.txt
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C7 H23 Co N5 O9.50 S2'
_cod_database_code               7011599