Trapping of anionic organic radicals by (TpMe2)2Ln (Ln = Sm, Eu).
Domingos, Angela; Lopes, Irene; Waerenborgh, João C; Marques, Noémia; Lin, G. Y.; Zhang, X. W.; Takats, Josef; McDonald, Robert; Hillier, Anna C.; Sella, Andrea; Elsegood, Mark R. J.; Day, Victor W.; Inorganic chemistry 46 (2007) 9415–9424; doi:10.1021/ic701364k

data_4338970
_publ_section_title
;
 Trapping of anionic organic radicals by (TpMe2)2Ln (Ln = Sm, Eu).
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9415
_journal_page_last               9424
_journal_paper_doi               10.1021/ic701364k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '2(C43 H54 B2 N12 O Sm), C7 H8'
_chemical_formula_sum            'C93 H116 B4 N24 O2 Sm2'
_chemical_formula_weight         1946.04
_chemical_name_systematic
;
 Bis(hydrido(tris-(3,5-dimethylpyrazolyl)borato)-
              samarium(III)benzophenone ketyl
;
_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                73.050(11)
_cell_angle_beta                 86.620(10)
_cell_angle_gamma                67.920(10)
_cell_formula_units_Z            1
_cell_length_a                   11.108(2)
_cell_length_b                   13.5320(19)
_cell_length_c                   17.7880(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      13.6
_cell_measurement_theta_min      7.3
_cell_volume                     2366.2(6)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MOLEN(Fair,1990)
_computing_molecular_graphics    ORTEP(Johnson,1976)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86(Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       \w-2\qscans
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8423
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.70
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.7222
_exptl_absorpt_correction_T_min  0.5825
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'empirical via \y-scan North et al (1968)'
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+3.7440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                6757
_reflns_number_total             7807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701364k-file001.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338970