Crystal structure of trihydrogen bis{[1,1,1-tris(2-oxidoethylaminomethyl)ethane]cobalt(III)} trinitrate
Sethi, Waqas; Johannesen, Heini V.; Morsing, Thorbjørn J.; Piligkos, Stergios; Weihe, Høgni; Acta Crystallographica Section E 71 (2015) m275–m276; doi:10.1107/S2056989015024664

data_2241508
_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
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>olex2.solve</i> (Bourhis <i>et al.</i>,  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       '\f and \w 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 <i>x</i> determined from
486 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</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/[\s^2^(Fo^2^)]
 where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            cv5501sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2472(3)
_cod_database_code               2241508
_shelx_estimated_absorpt_t_min   0.729
_shelx_estimated_absorpt_t_max   0.852
_shelx_hkl_checksum              54620
_shelx_res_checksum              98410
_shelxl_version_number           20.13
_cod_database_fobs_code 2241508