Facile synthesis of rare-earth pyrazolonates by the reaction of rare-earth metals with 1-phenyl-3-methyl-4-isobutyryl-5-pyrazolone. Crystal structures of [Ln(PMIP)3]2 (Ln = Y, Gd, Tb, Er, Tm)
Anastasia V. Safronova; Leonid N. Bochkarev; Irina P. Malysheva; Evgenii V. Baranov; Inorganica Chimica Acta 392 (2012) 454–458; doi:10.1016/j.ica.2012.03.032

data_1512656
_publ_section_title
;
 Facile synthesis of rare-earth pyrazolonates by the reaction of
 rare-earth metals with 1-phenyl-3-methyl-4-isobutyryl-5-pyrazolone.
 Crystal structures of [Ln(PMIP)3]2 (Ln = Y, Gd, Tb, Er, Tm)
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              454
_journal_page_last               458
_journal_paper_doi               10.1016/j.ica.2012.03.032
_journal_volume                  392
_journal_year                    2012
_chemical_formula_sum            'C84 H90 N12 O12 Tm2'
_chemical_formula_weight         1797.54
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.7530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5442(6)
_cell_length_b                   12.5911(6)
_cell_length_c                   23.4924(11)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     4001.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23770
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    2.271
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.4790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.811
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7851
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                5904
_reflns_number_total             7851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-454-458-5.cif
_cod_data_source_block           tmpmipm
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1512656