Crystal structures of two mononuclear complexes of terbium(III) nitrate with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane
Gregório, Thaiane; Giese, Siddhartha O. K.; Nunes, Giovana G.; Soares, Jaísa F.; Hughes, David L.; Acta Crystallographica Section E 73 (2017) 278–285; doi:10.1107/S2056989017001116

data_2242066
_publ_section_title
;
 Crystal structures of two mononuclear complexes of terbium(III) nitrate
 with the tripodal alcohol 1,1,1-tris(hydroxymethyl)propane
;
_journal_coeditor_code           HB7653
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              278
_journal_page_last               285
_journal_paper_doi               10.1107/S2056989017001116
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Tb (N O3)2 (C6 H14 O3)2] N O3, 0.5C4 H10 O2'
_chemical_formula_moiety         'C12 H28 N2 O12 Tb, N O3, C2 H5 O1'
_chemical_formula_structural     '[Tb(NO3)2(Tripodal)2][NO3].0.5(glyme)'
_chemical_formula_sum            'C14 H33 N3 O16 Tb'
_chemical_formula_weight         658.35
_chemical_name_systematic
;
Dinitratobis[1,1,1-tris(hydroxymethyl)propane]terbium(III) nitrate
dimethoxyethane hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.004(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1864(13)
_cell_length_b                   10.2997(6)
_cell_length_c                   23.832(2)
_cell_measurement_reflns_used    9404
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      3.07
_cell_volume                     4712.4(6)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
ORTEP (Johnson, 1976) and ORTEP-3 (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE/PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w 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  0.0707
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            172878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_min         2.662
_exptl_absorpt_coefficient_mu    3.083
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.538
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+5.6056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0341
_refine_ls_wR_factor_ref         0.0358
_reflns_number_gt                5031
_reflns_number_total             5889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7653sup1.cif
_cod_data_source_block           Compound-1
_cod_original_formula_sum        'C14 H33 N3 O16 Tb1'
_cod_database_code               2242066
_cod_database_fobs_code          2242066
_shelx_estimated_absorpt_t_min   0.669
_shelx_estimated_absorpt_t_max   0.762
_shelx_hkl_checksum              5678
_shelx_res_checksum              15397