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_4320818
_publ_contact_author_address
;       CEA, DCC/DRRV/SEMP/LCTS
        ValRho, BP 171
        30207 Bagnols-sur-C\`eze
        France
;
_publ_contact_author_email       denauwer@amandine.cea.fr
_publ_contact_author_fax         '33(4)66 79 65 31'
_publ_contact_author_name        'Mikhail Grigoriev'
_publ_contact_author_phone       '33(4)66 79 65 89'
_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            'C66 H132 N21 Nd3 O39'
_chemical_formula_weight         2276.65
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.572(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2627(4)
_cell_length_b                   20.5992(8)
_cell_length_c                   22.2126(8)
_cell_measurement_reflns_used    19573
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      2.7
_cell_volume                     5029.8(3)
_computing_cell_refinement       'HKL package (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD 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      273(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f 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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19573
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.615
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'translucent light pink'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Parallelepipedic
_exptl_crystal_F_000             2334
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1185
_refine_ls_number_reflns         10487
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.236
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+1.6997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1115
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                7992
_reflns_number_total             10487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990817x_2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0469P)^2^+1.6997P] 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^)+(0.0469P)^2^+1.6997P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5030(2)
_cod_database_code               4320818