Hydrolytic synthesis and structural characterization of lanthanide-acetylacetonato/hydroxo cluster complexes‒a systematic study.
Wu, Yinglan; Morton, Scott; Kong, Xiangjian; Nichol, Gary S.; Zheng, Zhiping; Dalton transactions (Cambridge, England : 2003) 40 (2011) 1041–1046; doi:10.1039/c0dt01218a

data_7014844
_publ_section_title
;
 Hydrolytic synthesis and structural characterization of
 lanthanide-acetylacetonato/hydroxo cluster complexes--a systematic
 study.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1041
_journal_page_last               1046
_journal_paper_doi               10.1039/c0dt01218a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C13 H21 O7 Pr'
_chemical_formula_sum            'C13 H21 O7 Pr'
_chemical_formula_weight         430.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.367(2)
_cell_angle_beta                 87.269(2)
_cell_angle_gamma                76.238(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9046(11)
_cell_length_b                   10.4942(17)
_cell_length_c                   12.242(2)
_cell_measurement_reflns_used    5395
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.99
_cell_measurement_theta_min      2.29
_cell_volume                     820.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 1999)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.784
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube with Miracol optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7987
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         33.99
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    2.995
_exptl_absorpt_correction_T_max  0.8671
_exptl_absorpt_correction_T_min  0.3626
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.233
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                4813
_reflns_number_total             5241
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0DT01218A.TXT
_cod_data_source_block           Pr2
_cod_database_code               7014844