Synthesis and thermal transformation of a neodymium(III) complex [Nd(HTBA)2(C2H3O2)(H2O)2].2H2O to noncentrosymmetric oxosulfate Nd2O2SO4
Golovnev, Nikolay; Molokeev, Maxim; Vereshchagin, Sergey; Atuchin, Victor; Journal of Coordination Chemistry 68 (2015) 1865–; doi:10.1080/00958972.2015.1031119

data_1529234
_publ_section_title
;
 Synthesis and thermal transformation of a neodymium(III) complex
 [Nd(HTBA)2(C2H3O2)(H2O)2].2H2O to noncentrosymmetric oxosulfate Nd2O2SO4
;
_journal_issue                   11
_journal_name_full               'Journal of Coordination Chemistry'
_journal_page_first              1865
_journal_paper_doi               10.1080/00958972.2015.1031119
_journal_volume                  68
_journal_year                    2015
_chemical_formula_moiety         'C10 H13 N4 Nd O8 S2, 2(H2 O)'
_chemical_formula_sum            'C10 H17 N4 Nd O10 S2'
_chemical_formula_weight         561.64
_chemical_name_systematic
;
Catena-Bis(mu~2~-2-thiobarbiturato-O,O')-(mu~3~-acetato-O,O,O')-
diaqua-neodymium(III) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.8380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5939(2)
_cell_length_b                   22.9953(5)
_cell_length_c                   10.1832(2)
_cell_measurement_temperature    296(2)
_cell_volume                     1854.64(7)
_computing_cell_refinement       'APEX2 (Bruker, 2003-2008)'
_computing_data_collection       'APEX2 (Bruker, 2003-2008)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18354
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    3.083
_exptl_absorpt_correction_T_max  0.8611
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1. Bruker AXS Inc., Madison, Wisconsin, USA, 2004
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.0975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0498
_reflns_number_gt                5051
_reflns_number_total             5416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NdHTBA2acetateH2O5.cif
_cod_data_source_block           f
_cod_original_sg_symbol_Hall
;
-P 2yn
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1529234
_cod_database_fobs_code          1529234