Solid-State and Solution Properties of Cationic Lanthanide Complexes of a New Neutral Heptadentate N4O3 Tripodal Ligand
Florence Bravard; Yann Bretonnière; Raphaël Wietzke; Christelle Gateau; Marinella Mazzanti; Pascale Delangle; Jacques Pécaut; Inorganic Chemistry 42 (2003) 7978–7989; doi:10.1021/ic034692e

data_4312608
_publ_section_title
;
 Solid-State and Solution Properties of Cationic Lanthanide Complexes of a
 New Neutral Heptadentate N4O3 Tripodal Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7978
_journal_page_last               7989
_journal_paper_doi               10.1021/ic034692e
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C71 H110 Cl9 N14 Nd3 O11'
_chemical_formula_weight         2087.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   17.4751(10)
_cell_length_b                   28.8954(17)
_cell_length_c                   17.7919(10)
_cell_measurement_temperature    193(2)
_cell_volume                     8984.0(9)
_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 0.886
_diffrn_measured_fraction_theta_max 0.886
_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  0.0754
_diffrn_reflns_av_sigmaI/netI    0.1549
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            35251
_diffrn_reflns_theta_full        29.61
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.036
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4220
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         11414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.095
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                5642
_reflns_number_total             11414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034692esi20030923_045655_1.cif
_cod_data_source_block           structure_[Nd(tpaam)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312608