A solid-state study of eight-coordinate lanthanide(iii) complexes (Ln = Eu, Gd, Tb, Dy) with 1-hydroxy-2-pyridinone
Tedeschi, Christine; Azéma, Joëlle; Gornitzka, Heinz; Tisnès, Pierre; Picard, Claude; Dalton Transactions  (2003) 1738–; doi:10.1039/b300159h

data_7012687
_publ_section_title
;
 A solid-state study of eight-coordinate lanthanide(iii) complexes (Ln
 = Eu, Gd, Tb, Dy) with 1-hydroxy-2-pyridinone
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1738
_journal_paper_doi               10.1039/b300159h
_journal_year                    2003
_chemical_formula_sum            'C20 H25 Gd N4 Na O12.5'
_chemical_formula_weight         701.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   14.1145(6)
_cell_length_b                   19.1011(7)
_cell_length_c                   19.2734(7)
_cell_measurement_reflns_used    5472
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      31.002
_cell_measurement_theta_min      2.559
_cell_volume                     5196.2(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38047
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    2.640
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.748330
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.031(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         12904
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.5168P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                9857
_reflns_number_total             12904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300159h.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        'C20 H25 Gd N4 Na O12.50'
_cod_database_code               7012687