Coordination and Reductive Chemistry of Tetraphenylborate Complexes of Trivalent Rare Earth Metallocene Cations, [(C5Me5)2Ln][(μ-Ph)2BPh2]
Matthew R. MacDonald; Joseph W. Ziller; William J. Evans; Inorganic Chemistry 50 (2011) 4092–4106; doi:10.1021/ic2000409

data_4324980
_publ_contact_author
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Professor William J. Evans
Department of Chemistry
1102 Natural Sciences II
University of California, Irvine
Irvine, CA 92697-2025
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_publ_contact_author_email       wevans@uci.edu
_publ_contact_author_fax         '1  949 824 2210'
_publ_contact_author_phone       '1  949 824 5174'
_publ_section_title
;
 Coordination and Reductive Chemistry of Tetraphenylborate Complexes of
 Trivalent Rare Earth Metallocene Cations, [(C5Me5)2Ln][(\m-Ph)2BPh2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4092
_journal_page_last               4106
_journal_paper_doi               10.1021/ic2000409
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C50 H62 B O2 Y'
_chemical_formula_weight         794.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 105.1600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3246(4)
_cell_length_b                   14.1253(6)
_cell_length_c                   15.5657(7)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.50
_cell_volume                     2191.07(16)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25745
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.8856
_exptl_absorpt_correction_T_min  0.7090
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0431P)^2^+0.4843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                4640
_reflns_number_total             5359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2000409_si_002_04.cif
_cod_data_source_block           mrm9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
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_cod_database_code               4324980