A 1:1 diastereoisomeric complex of <i>trans</i>-2-{[(<i>R</i>)-(+)-1-phenylethylamino]carbonyl}cyclohexanecarboxylic acid
Kazuyuki Takahashi; Taka-aki Okamura; Hitoshi Yamamoto; Norikazu Ueyama; Acta Crystallographica Section E 59 (2003) o1953–o1955; doi:10.1107/S160053680302573X

data_2202964
_publ_section_title
;A 1:1 diastereoisomeric complex of
 <i>trans</i>-2-{[(<i>R</i>)-(+)-1-phenylethylamino]carbonyl}cyclohexanecarboxylic
 acid
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1953
_journal_page_last               o1955
_journal_paper_doi               10.1107/S160053680302573X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C16 H21 N O3'
_chemical_formula_moiety         'C16 H21 N O3'
_chemical_formula_sum            'C16 H21 N O3'
_chemical_formula_weight         275.34
_chemical_name_systematic
;
trans-2-{[(R)-(+)-1-Phenylethylamino]carbonyl}cyclohexanecarboxylic
acid
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.456(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6306(6)
_cell_length_b                   15.3825(8)
_cell_length_c                   10.8903(6)
_cell_measurement_reflns_used    13296
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     1539.02(15)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection
;
PROCESS-AUTO (Rigaku Corporation, 1998)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 2000)
;
_computing_molecular_graphics
;
TEXSAN and Mercury (Bruno et al., 2002)
;
_computing_publication_material  'TEXSAN and Mercury'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6718
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         3662
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0647P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                3161
_reflns_number_total             3662
_reflns_threshold_expression     'I >2\s(I)'
_cod_data_source_file            wn6184.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2202964
_cod_database_fobs_code          2202964