Direct determination of absolute configuration of carboxylic acids by cyclooctapyrrole.
Lintuluoto, Juha M.; Nakayama, Kana; Setsune, Jun-ichiro; Chemical communications (Cambridge, England)  (2006) 3492–3494; doi:10.1039/b606228h

data_7113340
_publ_section_title
;
 Direct determination of absolute configuration of carboxylic acids by
 cyclooctapyrrole.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3492
_journal_page_last               3494
_journal_paper_doi               10.1039/b606228h
_journal_year                    2006
_chemical_formula_moiety         'C92 H104 N8 * 2(C4 H10 O)'
_chemical_formula_sum            'C100 H124 N8 O2'
_chemical_formula_weight         1470.07
_chemical_name_common
;
2,3,6,7,11,12,15,16,20,21,24,25,29,30,33,34-hexadecaethyl-
9,18,27, 36-tetraphenyl(32)octaphyrin-(1.0.1.0.1.0.1.0)
;
_chemical_name_systematic
;
2,3,6,7,11,12,15,16,20,21,24,25,29,30,33,34-hexadecaethyl-9,18,27,
36-tetraphenyl[32]octaphyrin-(1.0.1.0.1.0.1.0)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.829(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.381(2)
_cell_length_b                   19.5758(18)
_cell_length_c                   23.321(2)
_cell_measurement_reflns_used    5091
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.368
_cell_measurement_theta_min      2.278
_cell_volume                     8806.6(14)
_computing_cell_refinement       'Bruker SAINT+ ver. 6.45'
_computing_data_collection       'Bruker SAINT+ ver. 6.45'
_computing_data_reduction        'Bruker SAINT+ ver. 6.45'
_computing_molecular_graphics    'Bruker XSHELL ver. 4.02'
_computing_publication_material  'Bruker SHELXTL ver. 6.14'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23466
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2510
_reflns_number_gt                4373
_reflns_number_total             8797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606228h.txt
_cod_data_source_block           o4ph
_cod_original_cell_volume        8806.7(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113340