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_4338971
_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         'C43 H52 B2 N12 O Sm, C7 H8'
_chemical_formula_sum            'C50 H60 B2 N12 O Sm'
_chemical_formula_weight         1017.07
_chemical_name_systematic
; 
 Bis(hydrido(tris-(3,5-dimethylpyrazolyl)borato)samarium(III)fluorenone 
 ketyl
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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
_cell_angle_alpha                90.0000(10)
_cell_angle_beta                 92.542(5)
_cell_angle_gamma                90.0000(10)
_cell_formula_units_Z            4
_cell_length_a                   17.7840(11)
_cell_length_b                   12.6480(12)
_cell_length_c                   22.1080(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      7.7
_cell_volume                     4967.9(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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       '\w-2\q 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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7766
_diffrn_reflns_theta_full        23.96
_diffrn_reflns_theta_max         23.96
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        27.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_T_max  0.8088
_exptl_absorpt_correction_T_min  0.6655
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ' \y-scan North et al(1968)'
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         7485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.5660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                5393
_reflns_number_total             7485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701364k-file001.cif
_cod_data_source_block           commpound3
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4338971