#------------------------------------------------------------------------------
#$Date: 2016-01-22 06:08:37 +0200 (Fri, 22 Jan 2016) $
#$Revision: 174761 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/15/2241508.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_2241508
loop_
_publ_author_name
'Sethi, Waqas'
'Johannesen, Heini V.'
'Morsing, Thorbjørn J.'
'Piligkos, Stergios'
'Weihe, Høgni'
_publ_section_title
;
 Crystal structure of trihydrogen
 bis{[1,1,1-tris(2-oxidoethylaminomethyl)ethane]cobalt(III)} trinitrate
;
_journal_coeditor_code           CV5501
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m275
_journal_page_last               m276
_journal_paper_doi               10.1107/S2056989015024664
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Co2 (C11 H25.5 N3 O3)2] (N O3)3'
_chemical_formula_moiety         'C22 H51 Co2 N6 O6 3+, 3(N O3 -)'
_chemical_formula_sum            'C22 H51 Co2 N9 O15'
_chemical_formula_weight         799.57
_chemical_name_systematic
;
Trihydrogen bis{[1,1,1-tris(2-oxidoethylaminomethyl)ethane]cobalt(III)}
trinitrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2'
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.543(4)
_cell_length_b                   8.543(4)
_cell_length_c                   39.11(2)
_cell_measurement_reflns_used    6958
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.80
_cell_volume                     2472(2)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
olex2.solve (Bourhis et al.,  2015)
;
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            32729
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.060
_diffrn_reflns_theta_min         2.802
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       prism
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.430
_refine_ls_abs_structure_details
;
Flack x determined from
486 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   0.011(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1357
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.818
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0475
_reflns_number_gt                1263
_reflns_number_total             1357
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cv5501sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2472(3)
_cod_database_code               2241508
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.729
_shelx_estimated_absorpt_t_max   0.852
_shelxl_version_number           20.13
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.0000 0.0000 0.55889(2) 0.00936(12) Uani d 1 . .
O O1 0.17219(17) 0.19761(18) 0.53088(3) 0.0118(3) Uani d 1 . .
H H1 0.176(5) 0.194(3) 0.5089(3) 0.018 Uiso d 0.5 . .
C C5 0.0000 0.0000 0.67637(7) 0.0177(7) Uani d 1 . .
N N2 0.6667 0.3333 0.57385(6) 0.0116(5) Uani d 1 . .
O O2 0.54318(19) 0.3734(2) 0.57427(4) 0.0237(4) Uani d 1 . .
C C3 0.1892(3) 0.0424(3) 0.62458(4) 0.0143(4) Uani d 1 . .
H H3A 0.2763 0.1666 0.6304 0.017 Uiso calc 1 . .
H H3B 0.2231 -0.0352 0.6367 0.017 Uiso calc 1 . .
N N1 0.1977(2) 0.0158(2) 0.58647(4) 0.0115(3) Uani d 1 . .
H H1A 0.3088 0.1208 0.5781 0.014 Uiso calc 1 . .
C C2 0.2123(3) -0.1482(3) 0.57812(4) 0.0133(4) Uani d 1 . .
H H2A 0.1193 -0.2535 0.5900 0.016 Uiso calc 1 . .
H H2B 0.3295 -0.1298 0.5849 0.016 Uiso calc 1 . .
C C4 0.0000 0.0000 0.63662(7) 0.0130(6) Uani d 1 . .
C C1 0.1742(4) 0.3620(2) 0.53957(4) 0.0144(4) Uani d 1 . .
H H1B 0.0776 0.3682 0.5278 0.017 Uiso calc 1 . .
H H1C 0.2885 0.4659 0.5330 0.017 Uiso calc 1 . .
N N3 0.3333 0.6667 0.6667 0.0389(11) Uani d 1 . .
O O3 0.3333 0.5219(4) 0.6667 0.0790(12) Uani d 1 . .
H H5 -0.123(2) -0.032(3) 0.6841(4) 0.008(5) Uiso d 1 A -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'
Co Co 0.3494 0.9721 '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'
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
O1 Co1 O1 2 3 91.01(6)
O1 Co1 O1 2 . 91.01(6)
O1 Co1 O1 3 . 91.01(6)
O1 Co1 N1 2 2 89.92(7)
O1 Co1 N1 . 3 177.58(6)
O1 Co1 N1 . 2 86.74(7)
O1 Co1 N1 3 2 177.58(7)
O1 Co1 N1 2 . 177.58(7)
O1 Co1 N1 3 3 89.92(7)
O1 Co1 N1 3 . 86.74(7)
O1 Co1 N1 . . 89.92(7)
O1 Co1 N1 2 3 86.74(7)
N1 Co1 N1 . 3 92.37(7)
N1 Co1 N1 . 2 92.37(7)
N1 Co1 N1 2 3 92.37(7)
Co1 O1 H1 . . 124.2(19)
C1 O1 Co1 . . 110.61(11)
C1 O1 H1 . . 107(2)
C4 C5 H5 . . 107.8(10)
O2 N2 O2 2_655 . 119.982(8)
O2 N2 O2 3_665 . 119.984(8)
O2 N2 O2 2_655 3_665 119.983(8)
H3A C3 H3B . . 107.8
N1 C3 H3A . . 109.0
N1 C3 H3B . . 109.0
N1 C3 C4 . . 112.85(16)
C4 C3 H3A . . 109.0
C4 C3 H3B . . 109.0
Co1 N1 H1A . . 106.7
C3 N1 Co1 . . 116.71(12)
C3 N1 H1A . . 106.7
C2 N1 Co1 . . 106.72(11)
C2 N1 C3 . . 112.72(14)
C2 N1 H1A . . 106.7
N1 C2 H2A . . 110.5
N1 C2 H2B . . 110.5
N1 C2 C1 . 3 106.35(14)
H2A C2 H2B . . 108.7
C1 C2 H2A 3 . 110.5
C1 C2 H2B 3 . 110.5
C3 C4 C5 . . 107.78(11)
C3 C4 C5 2 . 107.78(11)
C3 C4 C5 3 . 107.78(11)
C3 C4 C3 . 2 111.11(11)
C3 C4 C3 3 2 111.11(11)
C3 C4 C3 3 . 111.11(11)
O1 C1 C2 . 2 107.19(14)
O1 C1 H1B . . 110.3
O1 C1 H1C . . 110.3
C2 C1 H1B 2 . 110.3
C2 C1 H1C 2 . 110.3
H1B C1 H1C . . 108.5
O3 N3 O3 3_565 2_665 120.000(3)
O3 N3 O3 2_665 . 119.999(4)
O3 N3 O3 3_565 . 120.001(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O1 2 1.9313(14)
Co1 O1 3 1.9313(14)
Co1 O1 . 1.9314(15)
Co1 N1 . 1.9511(17)
Co1 N1 3 1.9511(18)
Co1 N1 2 1.9511(17)
O1 H1 . 0.861(12)
O1 C1 . 1.436(2)
C5 C4 . 1.555(4)
C5 H5 . 0.987(18)
N2 O2 . 1.2612(16)
N2 O2 2_655 1.2612(16)
N2 O2 3_665 1.2612(16)
C3 H3A . 0.9700
C3 H3B . 0.9700
C3 N1 . 1.515(2)
C3 C4 . 1.543(2)
N1 H1A . 0.9800
N1 C2 . 1.503(3)
C2 H2A . 0.9700
C2 H2B . 0.9700
C2 C1 3 1.523(2)
C4 C3 3 1.543(2)
C4 C3 2 1.543(2)
C1 C2 2 1.523(2)
C1 H1B . 0.9700
C1 H1C . 0.9700
N3 O3 3_565 1.237(3)
N3 O3 . 1.237(3)
N3 O3 2_665 1.237(3)
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 H1 O1 6_556 0.861(12) 1.589(14) 2.445(2) 172(4) yes
N1 H1A O2 . 0.98 2.09 3.042(3) 163 yes
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_4
_geom_torsion
Co1 O1 C1 C2 2 36.7(2)
Co1 N1 C2 C1 3 41.38(17)
C3 N1 C2 C1 3 170.77(17)
N1 C3 C4 C5 . 170.42(11)
N1 C3 C4 C3 2 -71.71(18)
N1 C3 C4 C3 3 52.55(19)
C4 C3 N1 Co1 . 16.05(19)
C4 C3 N1 C2 . -108.00(16)

_cod_database_fobs_code 2241508
