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_7014846
_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         'C80 H121 O42 Tb9, 4 H2 O'
_chemical_formula_sum            'C80 H129 O46 Tb9'
_chemical_formula_weight         3241.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.8879(9)
_cell_length_b                   18.8879(9)
_cell_length_c                   15.3095(7)
_cell_measurement_reflns_used    4096
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.92
_cell_measurement_theta_min      2.53
_cell_volume                     5461.7(4)
_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    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27009
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    5.823
_exptl_absorpt_correction_T_max  0.7251
_exptl_absorpt_correction_T_min  0.6253
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Four molecules of water per asymmetric unit removed with SQUEEZE
;
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.177
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                3937
_reflns_number_total             5403
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0DT01218A.TXT
_cod_data_source_block           Tb9
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7014846