Evaluation of cobalt(III) tetramethylchiroporphyrin as an analytical reagent for the determination of enantiomer composition of primary amines and aziridines by 1H NMR spectroscopy
Jean-Pierre Simonato; Sabrina Chappellet; Jacques Pécaut; Paul Baret; Jean-Claude Marchon; New J. Chem. 25 (2001) 714–720; doi:10.1039/b100268f

data_7051106
_publ_section_title
;
 Evaluation of cobalt(III) tetramethylchiroporphyrin as an analytical
 reagent for the determination of enantiomer composition of primary
 amines and aziridines by 1H NMR spectroscopy
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              714
_journal_page_last               720
_journal_paper_doi               10.1039/b100268f
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C77 H83 Cl16 Co N6 O8'
_chemical_formula_weight         1846.62
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_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
_cell_angle_alpha                81.9830(10)
_cell_angle_beta                 71.16
_cell_angle_gamma                86.8630(10)
_cell_formula_units_Z            1
_cell_length_a                   11.64390(10)
_cell_length_b                   12.7731(2)
_cell_length_c                   15.5221(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2163.43(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0854
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10128
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            indigo
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_coef       0.0140(5)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.995
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         8318
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.994
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_obs          0.0632
_refine_ls_shift/esd_max         0.026
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.1085P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1702
_refine_ls_wR_factor_obs         0.1576
_reflns_number_observed          6546
_reflns_number_total             8318
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b100268f.txt
_cod_data_source_block           R_naphthyl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.1085P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w==1/[\s^2^(Fo^2^)+(0.1085P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2163.44(6)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7051106
_diffrn_temperature              193(2)