Crystallographic, X-ray Absorption, and IR Studies of Solid- and Solution-State Structures of Tris(nitrato)N,N,N',N'-Tetraethylmalonamide Complexes of Lanthanides. Comparison with the Americium Complex
C. Den Auwer; M. C. Charbonnel; M. G. B. Drew; M. Grigoriev; M. J. Hudson; P. B. Iveson; C. Madic; M. Nierlich; M. T. Presson; R. Revel; M. L. Russell; P. Thuéry; Inorganic Chemistry 39 (2000) 1487–1495; doi:10.1021/ic990817x

data_4320817
_publ_contact_author_address
;     CEA / Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       thuery@drecam.cea.fr
_publ_contact_author_fax         '16(1)69 08 66 40'
_publ_contact_author_name        'Pierre Thu\'ery'
_publ_contact_author_phone       '16(1)69 08 63 29'
_publ_section_title
;
 Crystallographic, X-ray Absorption, and IR Studies of Solid- and
 Solution-State Structures of Tris(nitrato)N,N,N',N'-Tetraethylmalonamide
 Complexes of Lanthanides. Comparison with the Americium Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1487
_journal_page_last               1495
_journal_paper_doi               10.1021/ic990817x
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C22 H44 N7 O13 Yb'
_chemical_formula_weight         787.68
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.35420(10)
_cell_length_b                   18.1148(2)
_cell_length_c                   19.7675(2)
_cell_measurement_reflns_used    19495
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      1.5
_cell_volume                     3349.59(6)
_computing_cell_refinement       'HKL package (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD software (Nonius, 1997)'
_computing_data_reduction        'HKL package (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'area detector'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19495
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.859
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Parallelepipedic
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.2780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0422
_refine_ls_wR_factor_ref         0.0411
_reflns_number_gt                5987
_reflns_number_total             6136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990817x_1.cif
_cod_data_source_block           yb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.2780P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.2780P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320817