Redetermination of diaquatris(4-oxopent-2-en-2-olato-κ^2^<i>O</i>,<i>O</i>')lanthanum(III)
Okawara, Toru; Ishihama, Kohei; Takehara, Kenji; Acta Crystallographica Section E 70 (2014) m258–m259; doi:10.1107/S1600536814013336

data_2239675
_publ_section_title
;
 Redetermination of
 diaquatris(4-oxopent-2-en-2-olato-\k^2^<i>O</i>,<i>O</i>')lanthanum(III)
;
_journal_coeditor_code           HB7216
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m258
_journal_page_last               m259
_journal_paper_doi               10.1107/S1600536814013336
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[La (C5 H7 O2)3 (H2 O)2]'
_chemical_formula_moiety         'C15 H25 La O8'
_chemical_formula_sum            'C15 H25 La O8'
_chemical_formula_weight         472.26
_chemical_name_systematic
;
Diaquatris(4-oxopent-2-en-2-olato-\k^2^<i>O</i>,<i>O</i>')lanthanum(III)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                96.614(2)
_cell_angle_beta                 100.601(2)
_cell_angle_gamma                114.325(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9245(12)
_cell_length_b                   10.6597(15)
_cell_length_c                   11.3727(15)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.53
_cell_volume                     946.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    '<i>ORTEP-3 for Windows</i> (Farrugia, 2012)'
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13810
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.409
_refine_ls_extinction_coef       0.0149(8)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.2713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                5068
_reflns_number_total             5213
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7216sup1.cif
_cod_data_source_block           I
_cod_database_code               2239675
_cod_database_fobs_code          2239675