Unprecedented Transformation of a Hydrotris(pyrazolyl)borate Ligand at a Metal Center: Synthesis and Rearrangement of the First Mixed Tp/Cp Lanthanide Complex, Sm(TpMe2)2(Cp)
I. Lopes; G. Y. Lin; A. Domingos; R. McDonald; N. Marques; J. Takats; Journal of the American Chemical Society 121 (1999) 8110–8111; doi:10.1021/ja984227u

data_4116507
_publ_section_title
;
 Unprecedented Transformation of a Hydrotris(pyrazolyl)borate Ligand at a
 Metal Center: Synthesis and Rearrangement of the First Mixed Tp/Cp
 Lanthanide Complex, Sm(TpMe2)2(Cp)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8110
_journal_page_last               8111
_journal_paper_doi               10.1021/ja984227u
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C53 H67 B2 N12 Sm'
_chemical_formula_weight         1044.16
_chemical_name_systematic
; 
 ? 
;
_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                103.464(2)
_cell_angle_beta                 106.315(2)
_cell_angle_gamma                90.169(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8344(11)
_cell_length_b                   15.8217(16)
_cell_length_c                   18.058(2)
_cell_measurement_reflns_used    5985
_cell_measurement_temperature    193(2)
_cell_volume                     2615.5(5)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_sigmaI/netI    0.1613
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14286
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.8941
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       plate
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.225
_refine_diff_density_min         -2.658
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         9880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                6447
_reflns_number_total             9880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja984227u_2.cif
_cod_data_source_block           C53H67B2N12Sm
_cod_database_code               4116507