On the Structure and Volumetric Properties of Solvated Lanthanoid(III) Ions in Amide Solutions.
Fuchs, Anna; Lundberg, Daniel; Warmińska, Dorota; Persson, Ingmar; The journal of physical chemistry. B 117 (2013) 8502–8511; doi:10.1021/jp310111j

data_1512129
_publ_section_title
;
 On the Structure and Volumetric Properties of Solvated Lanthanoid(III)
 Ions in Amide Solutions.
;
_journal_issue                   28
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              8502
_journal_page_last               8511
_journal_paper_doi               10.1021/jp310111j
_journal_volume                  117
_journal_year                    2013
_chemical_compound_source        'crystallized from dma solution'
_chemical_formula_moiety         'C32 H72 La N8 O8, 3(C F3 O3 S)'
_chemical_formula_sum            'C35 H72 F9 La N8 O17 S3'
_chemical_formula_weight         1283.13
_chemical_name_common            'octakis(dma)lanthanum(III) triflate'
_chemical_name_systematic
'octakis(dma)lanthanum(III) trifluoromethanesulfonate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.527(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6284(11)
_cell_length_b                   25.1469(15)
_cell_length_c                   17.7155(11)
_cell_measurement_reflns_used    7912
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      32.2165
_cell_measurement_theta_min      3.3210
_cell_volume                     5623.8(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'Crysalis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'SHELXL (Sheldrick, 2008)'
_computing_publication_material  'Diamond 2.1e (Brandenburg, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans at different \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_sigmaI/netI    0.1057
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32706
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'enhance (Mo) X-ray source'
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK, CrysAlis (2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_recrystallization_method dma
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.850
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1298
_refine_ls_number_reflns         18573
_refine_ls_number_restraints     851
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+26.7368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2309
_refine_ls_wR_factor_ref         0.2454
_reflns_number_gt                16022
_reflns_number_total             18573
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jp310111j_si_002.cif
_cod_data_source_block           x1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1512129