Synthetic Aspects of (C5H4SiMe3)3Ln Rare-Earth Chemistry: Formation of (C5H4SiMe3)3Lu via [(C5H4SiMe3)2Ln]+Metallocene Precursors
Peterson, Jeffrey K.; MacDonald, Matthew R.; Ziller, Joseph W.; Evans, William J.; Organometallics 32 (2013) 2625–; doi:10.1021/om400116d

data_4080717
_publ_contact_author
; 
Professor William J. Evans
Department of Chemistry
1102 Natural Sciences II
University of California, Irvine
Irvine, CA 92697-2025
;
_publ_section_title
;
 Synthetic Aspects of (C5H4SiMe3)3Ln Rare-Earth Chemistry: Formation of
 (C5H4SiMe3)3Lu via [(C5H4SiMe3)2Ln]+Metallocene Precursors
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2625
_journal_paper_doi               10.1021/om400116d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C52 H70 B Lu O3 Si2'
_chemical_formula_weight         985.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2012
_cell_angle_alpha                87.2680(7)
_cell_angle_beta                 76.6168(7)
_cell_angle_gamma                78.7567(7)
_cell_formula_units_Z            4
_cell_length_a                   13.8245(8)
_cell_length_b                   19.0919(12)
_cell_length_c                   19.5594(12)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.18
_cell_volume                     4925.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53364
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.087
_exptl_absorpt_coefficient_mu    2.092
_exptl_absorpt_correction_T_max  0.8629
_exptl_absorpt_correction_T_min  0.4683
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.110
_refine_diff_density_max         3.303
_refine_diff_density_min         -1.499
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         20051
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+25.2694P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16642
_reflns_number_total             20051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400116d_si_003.cif
_cod_data_source_block           mrm54
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not' 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_database_code               4080717
_shelx_estimated_absorpt_t_min   0.423
_shelx_estimated_absorpt_t_max   0.802
_shelxl_version_number           2012-9
_shelx_res_checksum              96869
_shelx_hkl_checksum              91433