Enantiomeric crystallization of (±)-trans-1,2-diaminocyclohexane under pressure
Cai, Weizhao; Katrusiak, Andrzej; CrystEngComm 13 (2011) 6742–; doi:10.1039/c1ce05553d

data_7206640
_publ_section_title
;
 Enantiomeric crystallization of (+-)-trans-1,2-diaminocyclohexane under
 pressure
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              6742
_journal_paper_doi               10.1039/c1ce05553d
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C6 H14 N2'
_chemical_formula_sum            'C6 H14 N2'
_chemical_formula_weight         114.19
_chemical_name_common            (+-)-trans-1,2-Diaminocyclohexane
_chemical_name_systematic
;
(+-)-trans-1,2-Diaminocyclohexane
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.345(8)
_cell_length_b                   5.150(7)
_cell_length_c                   7.558(10)
_cell_measurement_pressure       650000
_cell_measurement_reflns_used    1502
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      3.64
_cell_volume                     324.8(7)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2004)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2004)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.421
_diffrn_measured_fraction_theta_max 0.421
_diffrn_measurement_device_type  'Kuma KM4CCD \k geometry'
_diffrn_measurement_method
;HP omega scans - for more details see:
A. Budzianowski, A. Katrusiak in High-Pressure Crystallography
(Eds.: A. Katrusiak, P. F. McMillan),
Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168
;
_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  0.2199
_diffrn_reflns_av_sigmaI/netI    0.1497
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1502
_diffrn_reflns_theta_full        28.60
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Katrusiak, A. (2003). REDSHABS - Program for correcting
reflections intensities for DAC absorption, gasket shadowing
and sample crystal absorption. Adam Mickiewicz University, Pozna\'n.
Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             128
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         351
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0939
_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^)+(0.0517P)^2^+0.0252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1724
_reflns_number_gt                253
_reflns_number_total             351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05553d.txt
_cod_data_source_block           (+-)-trans-1,2-Diaminocyclohexane_0.65GPa
_cod_original_sg_symbol_Hall     'P 2 2ab '
_cod_database_code               7206640