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_2243682
_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], H2 O'
_chemical_formula_moiety         'H8 N3 O13 Tm, H2 O'
_chemical_formula_sum            'H10 N3 O14 Tm'
_chemical_formula_weight         445.04
_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                63.696(4)
_cell_angle_beta                 84.656(5)
_cell_angle_gamma                76.146(4)
_cell_formula_units_Z            2
_cell_length_a                   6.5782(4)
_cell_length_b                   9.5213(5)
_cell_length_c                   10.4848(6)
_cell_measurement_reflns_used    15951
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      36.88
_cell_measurement_theta_min      3.19
_cell_volume                     571.51(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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18549
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.498
_diffrn_reflns_theta_min         3.190
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.846
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(X-AREA; Stoe, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.586
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.918
_refine_ls_extinction_coef       0.0130(4)
_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   0.647
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.647
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0171
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0285
_refine_ls_wR_factor_ref         0.0289
_reflns_number_gt                3394
_reflns_number_total             4113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5589sup1.cif
_cod_data_source_block           TONi-2_223K
_cod_database_code               2243682
_cod_database_fobs_code          2243682
_shelx_hkl_checksum              4748
_shelx_res_checksum              88569