Conformation and crystal structures of 1-aminocyclohexaneacetic acid (β^3,3^Ac~6~c) in N-protected derivatives
Ahmad Wani, Naiem; Gupta, Vivek K.; Kant, Rajni; Aravinda, Subrayashastry; Rai, Rajkishor; Acta Crystallographica Section E 70 (2014) 272–277; doi:10.1107/S1600536814020777

data_2240032
_publ_section_title
;
 Conformation and crystal structures of 1-aminocyclohexaneacetic acid
 (\b^3,3^Ac~6~c) in N-protected derivatives
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              272
_journal_page_last               277
_journal_paper_doi               10.1107/S1600536814020777
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C13 H17 N3 O3'
_chemical_formula_moiety         'C13 H17 N3 O3'
_chemical_formula_sum            'C13 H17 N3 O3'
_chemical_formula_weight         263.30
_chemical_name_common            Pyr-beta-3,3-Ac6c-OH
_chemical_name_systematic
;
2-[1-(Pyrazine-2-amido)cyclohexyl]acetic acid
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.71350(10)
_cell_length_b                   10.53210(10)
_cell_length_c                   14.3907(2)
_cell_measurement_reflns_used    28796
_cell_measurement_temperature    291
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.66
_cell_volume                     1320.66(3)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      291
_diffrn_detector_area_resol_mean 16.1049
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Difraction Xcalibur, Sapphire3 CCD'
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0115
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            68869
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Crysalis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.262
_refine_ls_abs_structure_details
;
(Flack, 1983): 1585 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.2(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2878
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.4913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                2670
_reflns_number_total             2878
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2313sup1.cif
_cod_data_source_block           III
_cod_database_code               2240032
_cod_database_fobs_code          2240032