Linkage isomerism and C???H activation in an ytterbium(ii) tetraphenylborate
Deacon, Glen B.; Forsyth, Craig M.; Chemical Communications  (2002) 2522–; doi:10.1039/b208149k

data_7114262
_publ_section_title
;
 Linkage isomerism and C???H activation in an ytterbium(ii)
 tetraphenylborate
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2522
_journal_paper_doi               10.1039/b208149k
_journal_year                    2002
_chemical_formula_sum            'C34 H46 B N O Si2 Yb'
_chemical_formula_weight         724.75
_chemical_name_systematic
; 
[(bis(trimethylsilyl)amido)(tetrahydrofuran)
(eta6,eta1-tetraphenylborato)ytterbium(II)] 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1600(2)
_cell_length_b                   14.5302(2)
_cell_length_c                   16.3056(2)
_cell_measurement_temperature    173(2)
_cell_volume                     3354.84(8)
_computing_cell_refinement       'DENZO-SMN (Otwinoski and Minor, 1993)'
_computing_data_collection       'COLLECT (Nonius BV, 1994)'
_computing_data_reduction        'DENZO-SMN (Otwinoski and Minor, 1993)'
_computing_molecular_graphics    'POVRAY 3.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Enraf Nonius KAPPA CCD'
_diffrn_measurement_method       '1 deg scans in phi and omega'
_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  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46392
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    2.885
_exptl_absorpt_process_details   none
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.395
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7833
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                5736
_reflns_number_total             7833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208149k.txt
_cod_data_source_block           1b
_cod_original_cell_volume        3354.8(12)
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7114262