#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/95/2019572.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019572
loop_
_publ_author_name
'Neis, Christian'
'Kradolfer, Thomas'
'Hegetschweiler, Kaspar'
_publ_section_title
;
 Formation of lithium, sodium and potassium complexes with
 1,3,5-triamino-1,3,5-trideoxy-cis-inositol (taci)
;
_journal_coeditor_code           CU3054
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              632
_journal_page_last               637
_journal_paper_doi               10.1107/S2053229614011036
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Na (C6 H15 N3 O3)2] I'
_chemical_formula_moiety         'C12 H30 N6 Na O6 +, I-'
_chemical_formula_sum            'C12 H30 I N6 Na O6'
_chemical_formula_weight         504.31
_chemical_name_systematic
'Bis(1,3,5-triamino-1,3,5-trideoxy-cis-inositol-κ³O²,O⁴,O⁶)sodium(I) iodide'
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.9637(6)
_cell_length_b                   10.9637(6)
_cell_length_c                   14.3641(8)
_cell_measurement_reflns_used    4773
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      33.17
_cell_measurement_theta_min      2.57
_cell_volume                     1495.28(14)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker Nonius X8 APEX diffractometer with Kappa CCD area detector'
_diffrn_measurement_method       'φ and ω 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  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0096
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3194
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_T_max  0.6345
_exptl_absorpt_correction_T_min  0.3637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         733
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0117
_refine_ls_R_factor_gt           0.0117
_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)+(0.0179P)²+1.6340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0340
_reflns_number_gt                733
_reflns_number_total             733
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cu3054sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2019570--2019572.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2019572
_cod_database_fobs_code          2019572
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
I I1 0.0000 0.0000 0.5000 0.01250(8) Uani d S 1 6
O O1 0.36478(9) 0.52714(9) 0.55261(6) 0.01095(17) Uani d D 1 1
H H1O 0.3686(18) 0.4532(16) 0.5593(11) 0.016 Uiso d D 1 1
C C1 0.21533(12) 0.52260(12) 0.42414(8) 0.0095(2) Uani d . 1 1
H H1 0.2140 0.5211 0.3545 0.011 Uiso calc R 1 1
Na Na1 0.3333 0.6667 0.6667 0.0112(2) Uani d S 1 6
N N2 0.09847(11) 0.38616(11) 0.45561(8) 0.0129(2) Uani d D 1 1
H H2B 0.109(2) 0.381(2) 0.5164(9) 0.019 Uiso d D 1 1
H H2A 0.1036(19) 0.3156(16) 0.4309(12) 0.019 Uiso d D 1 1
C C2 0.36015(12) 0.54690(12) 0.45451(8) 0.0094(2) Uani d . 1 1
H H2 0.3761 0.4752 0.4223 0.011 Uiso calc R 1 1
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 O1 Na1 . . 123.57(7) y
C2 O1 H1O . . 106.4(11) ?
Na1 O1 H1O . . 129.4(11) ?
N2 C1 C2 . 3_565 109.04(9) ?
N2 C1 C2 . . 112.83(9) ?
C2 C1 C2 3_565 . 113.65(11) ?
N2 C1 H1 . . 107.0 ?
C2 C1 H1 3_565 . 107.0 ?
C2 C1 H1 . . 107.0 ?
O1 Na1 O1 15_556 3_565 180.0 y
O1 Na1 O1 15_556 2_665 102.13(3) y
O1 Na1 O1 3_565 2_665 77.88(3) y
O1 Na1 O1 15_556 . 102.13(3) ?
O1 Na1 O1 3_565 . 77.88(3) ?
O1 Na1 O1 2_665 . 77.88(3) ?
O1 Na1 O1 15_556 14_456 77.88(3) ?
O1 Na1 O1 3_565 14_456 102.12(3) ?
O1 Na1 O1 2_665 14_456 180.0 ?
O1 Na1 O1 . 14_456 102.13(3) ?
O1 Na1 O1 15_556 13_566 77.87(3) ?
O1 Na1 O1 3_565 13_566 102.12(3) ?
O1 Na1 O1 2_665 13_566 102.12(3) ?
O1 Na1 O1 . 13_566 180.00(4) ?
O1 Na1 O1 14_456 13_566 77.87(3) ?
C1 N2 H2B . . 106.9(13) ?
C1 N2 H2A . . 111.4(12) ?
H2B N2 H2A . . 106.0(17) ?
O1 C2 C1 . 2_665 111.35(9) ?
O1 C2 C1 . . 111.44(9) ?
C1 C2 C1 2_665 . 110.83(11) ?
O1 C2 H2 . . 107.7 ?
C1 C2 H2 2_665 . 107.7 ?
C1 C2 H2 . . 107.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C2 . 1.4303(13) ?
O1 Na1 . 2.3813(8) y
O1 H1O . 0.838(14) ?
C1 N2 . 1.4721(15) ?
C1 C2 3_565 1.5309(15) ?
C1 C2 . 1.5359(15) ?
C1 H1 . 1.0000 ?
Na1 O1 15_556 2.3813(9) ?
Na1 O1 3_565 2.3813(8) ?
Na1 O1 2_665 2.3813(9) ?
Na1 O1 14_456 2.3813(9) ?
Na1 O1 13_566 2.3814(8) ?
N2 H2B . 0.885(13) ?
N2 H2A . 0.879(14) ?
C2 C1 2_665 1.5309(15) ?
C2 H2 . 1.0000 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1O N2 11_556 0.838(14) 1.930(14) 2.7525(14) 166.7(16) y
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C2 O1 Na1 O1 . 15_556 -140.07(6)
C2 O1 Na1 O1 . 3_565 39.93(7)
C2 O1 Na1 O1 . 2_665 -40.07(7)
C2 O1 Na1 O1 . 14_456 139.93(7)
Na1 O1 C2 C1 . 2_665 62.32(11)
Na1 O1 C2 C1 . . -61.98(11)
N2 C1 C2 O1 . . -52.73(13)
C2 C1 C2 O1 3_565 . 72.07(12)
N2 C1 C2 C1 . 2_665 -177.34(8)
C2 C1 C2 C1 3_565 2_665 -52.53(15)
