Differentiating Chemically Similar Lewis Acid Sites in Heterobimetallic Complexes: The Rare-Earth Bridged Hydride (C5Me5)2Ln(μ-H)2Ln′(C5Me5)2and Tuckover Hydride (C5Me5)2Ln(μ-H)(μ-η1:η5-CH2C5Me4)Ln′(C5Me5) Systems
Fieser, Megan E.; Mueller, Thomas J.; Bates, Jefferson E.; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Organometallics 33 (2014) 3882–; doi:10.1021/om500624x

data_4083926
_publ_section_title
;
 Differentiating Chemically Similar Lewis Acid Sites in Heterobimetallic
 Complexes: The Rare-Earth Bridged Hydride
 (C5Me5)2Ln(\m-H)2Ln&#x2032;(C5Me5)2and Tuckover Hydride
 (C5Me5)2Ln(\m-H)(\m-\h1:\h5-CH2C5Me4)Ln&#x2032;(C5Me5) Systems
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3882
_journal_paper_doi               10.1021/om500624x
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C40 H60 La Lu'
_chemical_formula_weight         854.76
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                102.7526(9)
_cell_angle_beta                 102.0384(9)
_cell_angle_gamma                99.3623(9)
_cell_formula_units_Z            2
_cell_length_a                   10.4850(8)
_cell_length_b                   10.8635(8)
_cell_length_c                   17.1425(13)
_cell_measurement_reflns_used    5283
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      2.50
_cell_volume                     1817.4(2)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART 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  0.0322
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19900
_diffrn_reflns_point_group_measured_fraction_full 0.997
_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         1.970
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.884
_exptl_absorpt_correction_T_max  0.8862
_exptl_absorpt_correction_T_min  0.5662
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.063
_refine_diff_density_max         5.932
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+17.7663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5788
_reflns_number_total             7409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500624x_si_002.cif
_cod_data_source_block           mef13
_cod_depositor_comments
;Adding full bibliography for 4083925--4083926.cif.

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 
;
_cod_database_code               4083926
_shelx_estimated_absorpt_t_min   0.461
_shelx_estimated_absorpt_t_max   0.792
_shelxl_version_number           2013-3
_shelx_res_checksum              44621
_shelx_hkl_checksum              54495