Crystal structures of the penta- and hexahydrate of thulium nitrate
Klein, Wilhelm; Acta Crystallographica Section E 76 (2020) 1863–1867; doi:10.1107/S2056989020015388

data_2243683
_publ_section_title
;
 Crystal structures of the penta- and hexahydrate of thulium nitrate
;
_journal_coeditor_code           WM5589
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1863
_journal_page_last               1867
_journal_paper_doi               10.1107/S2056989020015388
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '[Tm (N O3)3 (H2 O)4], 2H2 O'
_chemical_formula_moiety         'H8 N3 O13 Tm, 2(H2 O)'
_chemical_formula_sum            'H12 N3 O15 Tm'
_chemical_formula_weight         463.06
_chemical_name_systematic
;
Thulium nitrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                70.924(4)
_cell_angle_beta                 88.908(4)
_cell_angle_gamma                68.923(4)
_cell_formula_units_Z            2
_cell_length_a                   6.7050(3)
_cell_length_b                   8.9733(4)
_cell_length_c                   11.4915(6)
_cell_measurement_reflns_used    47483
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      36.56
_cell_measurement_theta_min      2.59
_cell_volume                     605.90(6)
_computing_cell_refinement
;
X-AREA (Stoe, 2015)
;
_computing_data_collection
;
X-AREA (Stoe, 2015)
;
_computing_data_reduction
;
X-AREA (Stoe, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      223(2)
_diffrn_detector                 STOE
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.412
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(X-AREA; Stoe, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.538
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.185
_refine_ls_extinction_coef       0.0687(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0342
_refine_ls_wR_factor_ref         0.0345
_reflns_number_gt                3899
_reflns_number_total             4385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5589sup1.cif
_cod_data_source_block           TONii-3_223K
_cod_original_cell_volume        605.90(5)
_cod_database_code               2243683
_cod_database_fobs_code          2243683
_shelx_hkl_checksum              15584
_shelx_res_checksum              85894