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_4318611
_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_moiety         '[SmL](EtOH).2.5H2O'
_chemical_formula_sum            'C28 H41 N6 O11.5 Sm'
_chemical_formula_weight         796.02
_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                 97.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.163(3)
_cell_length_b                   19.329(4)
_cell_length_c                   17.371(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3384.7(16)
_computing_cell_refinement       'CAD4-Express Software (Nonius, 1994)'
_computing_data_collection       'CAD4-Express Software (Nonius, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'MACH3 Enraf Nonius'
_diffrn_measurement_method       omega
_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  0.0815
_diffrn_reflns_av_sigmaI/netI    0.2322
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10724
_diffrn_reflns_theta_full        30.41
_diffrn_reflns_theta_max         30.41
_diffrn_reflns_theta_min         2.11
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.801
_exptl_absorpt_correction_T_max  0.8693
_exptl_absorpt_correction_T_min  0.6718
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.00091(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         10214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.2128
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0840P)^2^+7.2436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1960
_reflns_number_gt                4925
_reflns_number_total             10214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0257017_s3.cif
_cod_data_source_block           smn
_cod_original_cell_volume        3384.8(14)
_cod_original_formula_sum        'C28 H41 N6 O11.50 Sm'
_cod_database_code               4318611