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_7011598
_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         'C6 H18 Co N5 O2, 2Br, H2O'
_chemical_formula_sum            'C6 H20 Br2 Co N5 O3'
_chemical_formula_weight         429.02
_chemical_name_systematic
; 
LAMBDA(+)578-[(en)2Co(O2CCH=NH)]Br2,H2O
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1300(2)
_cell_length_b                   8.3730(3)
_cell_length_c                   20.9660(6)
_cell_measurement_reflns_used    172
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      23.9
_cell_measurement_theta_min      3.2
_cell_volume                     1427.21(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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30189
_diffrn_reflns_theta_full        35.01
_diffrn_reflns_theta_max         35.01
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    6.807
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_correction_T_min  0.167
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.124
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.212
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.032(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         6211
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0184P)^2^+10.0960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                5893
_reflns_number_total             6211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202090d.txt
_cod_data_source_block           9
_cod_database_code               7011598