Anionic lanthanide complexes with 3-methyl-1-phenyl-4-formylpyrazole-5-one and hydroxonium as counter ion
Victor F. Shul-gin; Oleg V. Konnik; Susana V. Abkhairova; Alexey N. Gusev; Svetlana B. Meshkova; Anna V. Kiriyak; Eduard B. Rusanov; Miki Hasegawa; Wolfgang Linert; Inorganica Chimica Acta 402 (2013) 33–38; doi:

data_1517045
_publ_section_title
;
 Anionic lanthanide complexes with
 3-methyl-1-phenyl-4-formylpyrazole-5-one and hydroxonium as counter ion
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              33
_journal_page_last               38
_journal_volume                  402
_journal_year                    2013
_chemical_formula_sum            'C44 H41 N8 O10 Sm'
_chemical_formula_weight         992.20
_chemical_name_systematic
; 
Hydroxonium 
Tetrakis(3-methyl-1-phenyl-4-formylpyrazole-5-onato)samarium(III)ate
;
_space_group_IT_number           120
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2701(4)
_cell_length_b                   16.2701(4)
_cell_length_c                   16.1315(6)
_cell_measurement_temperature    296(2)
_cell_volume                     4270.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1090
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26102
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.444
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2012
_refine_diff_density_max         1.881
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+8.6518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                1822
_reflns_number_total             2616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-402-33-38-2.cif
_cod_data_source_block           06
_cod_original_sg_symbol_H-M      I-4c2
_cod_database_code               1517045