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_4115770
_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            'C59 H75.5 Cl4 Co N6 O14.25'
_chemical_formula_weight         1297.48
_chemical_name_systematic
;
 ?
;
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.581(4)
_cell_angle_beta                 77.543(4)
_cell_angle_gamma                75.193(4)
_cell_formula_units_Z            2
_cell_length_a                   13.240(3)
_cell_length_b                   13.960(3)
_cell_length_c                   19.037(4)
_cell_measurement_temperature    193(2)
_cell_volume                     3192.4(12)
_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 0.866
_diffrn_measured_fraction_theta_max 0.866
_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  0.0914
_diffrn_reflns_av_sigmaI/netI    0.5062
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20131
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.503
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_exptl_crystal_F_000             1361
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.687
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         17167
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_refine_ls_R_factor_all          0.2642
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.2150
_reflns_number_gt                4915
_reflns_number_total             17167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016494x_s2_3.cif
_cod_data_source_block           Rthr
_cod_original_cell_volume        3192.5(10)
_cod_original_formula_sum        'C59 H75.50 Cl4 Co N6 O14.25'
_cod_database_code               4115770