Synthetic Utility of [(C5Me5)2Ln][(μ-Ph)2BPh2] in Accessing [(C5Me5)2LnR]x Unsolvated Alkyl Lanthanide Metallocenes, Complexes with High C-H Activation Reactivity
William J. Evans; Jeremy M. Perotti; Joseph W. Ziller; Journal of the American Chemical Society 127 (2005) 3894–3909; doi:10.1021/ja045064e

data_4111541
_publ_section_title
;
 Synthetic Utility of [(C5Me5)2Ln][(\m-Ph)2BPh2] in Accessing
 [(C5Me5)2LnR]x Unsolvated Alkyl Lanthanide Metallocenes, Complexes with
 High C-H Activation Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3894
_journal_page_last               3909
_journal_paper_doi               10.1021/ja045064e
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C50 H82 O4 Si2 Sm2'
_chemical_formula_weight         1104.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.523(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   32.132(3)
_cell_length_b                   21.368(2)
_cell_length_c                   23.512(2)
_cell_measurement_temperature    163(2)
_cell_volume                     15554(2)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            78827
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_T_max  0.7070
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6792
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         17158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+83.6448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                12420
_reflns_number_total             17158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045064esi20041209_060807.cif
_cod_data_source_block           jp42
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        15555(3)
_cod_database_code               4111541