X-ray Diffraction and 1H NMR in Solution: Structural Determination of Lanthanide Complexes of a Py2N6Ac4 Ligand
L. Valencia; J. Martinez; A. Macías; R. Bastida; R. A. Carvalho; C. F. G. C. Geraldes; Inorganic Chemistry 41 (2002) 5300–5312; doi:10.1021/ic0257017

data_4318610
_publ_section_title
;
 X-ray Diffraction and 1H NMR in Solution: Structural Determination of
 Lanthanide Complexes of a Py2N6Ac4 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5300
_journal_page_last               5312
_journal_paper_doi               10.1021/ic0257017
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C26 H30 La N7 O15'
_chemical_formula_weight         819.48
_chemical_name_systematic
;
 ?
;
_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                 92.3040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7586(5)
_cell_length_b                   19.5753(10)
_cell_length_c                   16.6679(8)
_cell_measurement_temperature    173(2)
_cell_volume                     3181.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19193
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.426
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1648
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                5720
_reflns_number_total             7389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0257017_s2.cif
_cod_data_source_block           lan
_cod_database_code               4318610