Three-Point versus Two-Point Attachment of (R)- and (S)-Amino Acid Methyl Esters to a Cobalt(III) Chiroporphyrin: Implications for the Analysis of Amino Acid Enantiomers by 1H NMR Spectroscopy
Magalie Claeys-Bruno; Dawn Toronto; Jacques Pécaut; Michel Bardet; Jean-Claude Marchon; Journal of the American Chemical Society 123 (2001) 11067–11068; doi:10.1021/ja016494x

data_4115772
_publ_section_title
;
 Three-Point versus Two-Point Attachment of (R)- and (S)-Amino Acid Methyl
 Esters to a Cobalt(III) Chiroporphyrin: Implications for the Analysis of
 Amino Acid Enantiomers by 1H NMR Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11067
_journal_page_last               11068
_journal_paper_doi               10.1021/ja016494x
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C66 H82 Cl13 Co N6 O16'
_chemical_formula_weight         1735.16
_chemical_name_systematic
;
 ?
;
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_symmetry_cell_setting           orthorhombic
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0919(7)
_cell_length_b                   19.9345(8)
_cell_length_c                   23.5472(8)
_cell_measurement_temperature    193(2)
_cell_volume                     8023.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.870
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.1233
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_k_min       -26
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33152
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         18983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                10127
_reflns_number_total             18983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016494x_s2_5.cif
_cod_data_source_block           Sglu
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