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_4318616
_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            'C28 H30 N6 O11 Tm'
_chemical_formula_weight         795.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.2933(12)
_cell_length_b                   14.3595(16)
_cell_length_c                   39.380(4)
_cell_measurement_temperature    173(2)
_cell_volume                     6386.1(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.1250
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            35732
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    2.846
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3176
_refine_diff_density_max         2.228
_refine_diff_density_min         -9.170
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_gt           0.1169
_refine_ls_shift/su_max          0.941
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+225.8277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2424
_reflns_number_gt                4754
_reflns_number_total             7642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0257017_s8.cif
_cod_data_source_block           tmn
_cod_database_code               4318616