Controlled Hydrolysis of Lanthanide Complexes of the N-Donor Tripod Tris(2-pyridylmethyl)amine versus Bisligand Complex Formation
Louise Natrajan; Jacques Pécaut; Marinella Mazzanti; Colette LeBrun; Inorganic Chemistry 44 (2005) 4756–4765; doi:10.1021/ic0502224

data_4309108
_publ_section_title
;
Controlled Hydrolysis of Lanthanide Complexes of the N-Donor Tripod
Tris(2-pyridylmethyl)amine versus Bisligand Complex Formation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4756
_journal_page_last               4765
_journal_paper_doi               10.1021/ic0502224
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H37.65 Eu F9 N8.5 O9.08 S3'
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_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.057(3)
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_cell_length_c                   23.605(4)
_cell_measurement_temperature    193(2)
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_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
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_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42972
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4814
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         13831
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+13.9656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                11980
_reflns_number_total             13831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0502224si20050211_013138_6.cif
_cod_data_source_block           struc_Eu(tpa)2(Otf)3,6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        9657(3)
_cod_original_formula_sum        'C40 H37.65 Eu F9 N8.50 O9.08 S3'
_cod_database_code               4309108