#------------------------------------------------------------------------------
#$Date: 2016-02-14 05:40:26 +0100 (dom 14 de feb de 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/66/7206639.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7206639
loop_
_publ_author_name
'Cai, Weizhao'
'Katrusiak, Andrzej'
_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                   8.40(6)
_cell_length_b                   5.159(5)
_cell_length_c                   7.61(3)
_cell_measurement_pressure       520000
_cell_measurement_reflns_used    1837
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      4.77
_cell_volume                     330(3)
_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 0.348
_diffrn_measured_fraction_theta_max 0.348
_diffrn_measurement_device_type  'Kuma KM4CCD κ 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  0.3243
_diffrn_reflns_av_sigmaI/netI    0.3488
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1837
_diffrn_reflns_theta_full        28.80
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         4.77
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.80
_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, Poznań.
Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             128
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         300
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.4255
_refine_ls_R_factor_gt           0.1889
_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/[σ²(Fo²)+(0.1515P)²+0.3990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3133
_refine_ls_wR_factor_ref         0.4550
_reflns_number_gt                82
_reflns_number_total             300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05553d.txt
_cod_data_source_block           (+-)-trans-1,2-Diaminocyclohexane_0.52GPa
_cod_original_sg_symbol_Hall     'P 2 2ab '
_cod_database_code               7206639
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
N1 N 0.629(3) 0.187(3) 1.0044(16) 0.078(7) Uiso 1 1 d G
H1 H 0.5720 0.1311 1.0877 0.093 Uiso 1 1 d GD
H2 H 0.7020 0.2952 1.0223 0.093 Uiso 1 1 d GD
C1 C 0.540(4) 0.140(4) 0.853(2) 0.074(7) Uiso 1 1 d D
H3 H 0.4530 0.2673 0.8511 0.088 Uiso 1 1 calc R
C2 C 0.630(4) 0.166(4) 0.683(2) 0.066(11) Uani 1 1 d .
H4 H 0.7141 0.0381 0.6820 0.079 Uiso 1 1 calc R
H5 H 0.6798 0.3358 0.6811 0.079 Uiso 1 1 calc R
C3 C 0.537(3) 0.137(4) 0.519(2) 0.072(10) Uani 1 1 d .
H6 H 0.4538 0.2672 0.5137 0.087 Uiso 1 1 calc R
H7 H 0.6058 0.1585 0.4178 0.087 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C2 0.08(4) 0.060(10) 0.060(19) -0.017(14) -0.027(16) -0.013(15)
C3 0.04(4) 0.081(12) 0.10(2) 0.010(16) 0.022(14) 0.018(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 N1 H1 104.7 . .
C1 N1 H2 129.9 . .
H1 N1 H2 121.1 . .
N1 C1 C1 112.5(15) . 2_655
N1 C1 C2 115(2) . .
C1 C1 C2 107.0(14) 2_655 .
N1 C1 H3 107.3 . .
C1 C1 H3 107.3 2_655 .
C2 C1 H3 107.3 . .
C3 C2 C1 117(3) . .
C3 C2 H4 108.1 . .
C1 C2 H4 108.1 . .
C3 C2 H5 108.1 . .
C1 C2 H5 108.1 . .
H4 C2 H5 107.3 . .
C2 C3 C3 107.8(14) . 2_655
C2 C3 H6 110.1 . .
C3 C3 H6 110.1 2_655 .
C2 C3 H7 110.1 . .
C3 C3 H7 110.1 2_655 .
H6 C3 H7 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.40(3) .
N1 H1 0.8457 .
N1 H2 0.8400 .
C1 C1 1.59(5) 2_655
C1 C2 1.51(3) .
C1 H3 0.9800 .
C2 C3 1.48(2) .
C2 H4 0.9700 .
C2 H5 0.9700 .
C3 C3 1.54(5) 2_655
C3 H6 0.9700 .
C3 H7 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 C1 C2 C3 -175.8(18) . .
C1 C1 C2 C3 58(3) 2_655 .
C1 C2 C3 C3 -60(3) . 2_655
