Lanthanide and Uranium Complexes with an SPS-Based Pincer Ligand
Arliguie, Thérèse; Doux, Marjolaine; Mézailles, Nicolas; Thuéry, Pierre; Le Floch, Pascal; Ephritikhine, Michel; Inorganic Chemistry 45 (2006) 9907–9913; doi:10.1021/ic061364g

data_4333073
_publ_section_title
;
 Lanthanide and Uranium Complexes with an SPS-Based Pincer Ligand
;
_journal_issue                   24
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9907
_journal_page_last               9913
_journal_paper_doi               10.1021/ic061364g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C56 H70 B2 Ce O3.5 P3 S2'
_chemical_formula_weight         1117.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.174(3)
_cell_angle_beta                 91.414(3)
_cell_angle_gamma                98.993(4)
_cell_formula_units_Z            4
_cell_length_a                   10.3250(4)
_cell_length_b                   22.8023(14)
_cell_length_c                   23.9332(14)
_cell_measurement_reflns_used    37405
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      4.11
_cell_volume                     5538.4(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f 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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.1137
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37405
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         4.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.678
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         19245
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0723
_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^)+(0.0445P)^2^+28.9049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1743
_reflns_number_gt                12267
_reflns_number_total             19245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061364gsup1.cif
_cod_data_source_block           1.1.5thf
_cod_original_formula_sum        'C56 H70 B2 Ce O3.50 P3 S2'
_cod_database_code               4333073