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_4116506
_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_structural     Sm[HB(3,5-Me2pz)2(C5H4)](TpMe2)
_chemical_formula_sum            'C33.5 H45 B2 N10 Sm'
_chemical_formula_weight         759.77
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.725(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3256(9)
_cell_length_b                   20.008(2)
_cell_length_c                   21.468(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      7.6
_cell_volume                     3568.6(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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4-Enraf Nonius'
_diffrn_measurement_method       '\w/2\q scan'
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6292
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        6.7
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.6833
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.106
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5356
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.562
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_obs          0.0653
_refine_ls_shift/esd_max         0.120
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+36.5780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2281
_refine_ls_wR_factor_obs         0.1360
_reflns_number_observed          4313
_reflns_number_total             6124
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja984227u_1.cif
_cod_data_source_block           C33.50H45B2N10Sm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+36.5780P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+36.5780P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C33.50 H45 B2 N10 Sm'
_cod_database_code               4116506