Synthesis, Structures, and Magnetic and Optical Properties of a Series of Europium(III) and Gadolinium(III) Complexes with Chelating Nitronyl and Imino Nitroxide Free Radicals
Christophe Lescop; Dominique Luneau; Paul Rey; Guillaume Bussière; Christian Reber; Inorganic Chemistry 41 (2002) 5566–5574; doi:10.1021/ic0257928

data_4318728
_publ_contact_author
;
       Dominique LUNEAU
       Laboratoire de Chimie Inorganique et Biologique (UMR 5046)
       DRFMC
       CEA-Grenoble
       38054 Grenoble, France
;
_publ_contact_author_email       luneau@drfmc.ceng.cea.fr
_publ_contact_author_fax         '33 438 785 090'
_publ_contact_author_phone       '33 438 784 462'
_publ_section_title
;
 Synthesis, Structures, and Magnetic and Optical Properties of a Series of
 Europium(III) and Gadolinium(III) Complexes with Chelating Nitronyl and
 Imino Nitroxide Free Radicals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5566
_journal_page_last               5574
_journal_paper_doi               10.1021/ic0257928
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C29 H20 F18 Gd N4 O7'
_chemical_formula_weight         1035.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 108.795(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4160(14)
_cell_length_b                   21.877(3)
_cell_length_c                   16.1879(19)
_cell_measurement_temperature    193(2)
_cell_volume                     3827.3(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1044
_diffrn_reflns_av_sigmaI/netI    0.1371
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24449
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.869
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.545
_refine_diff_density_min         -2.317
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.144
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                5313
_reflns_number_total             9246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0257928_5.cif
_cod_data_source_block           cl402b_compound_3a
_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 
;
_cod_original_cell_volume        3827.4(8)
_cod_database_code               4318728