Reactivity of the Y3+Tuck-Over Hydride Complex, (C5Me5)2Y(μ-H)(μ-CH2C5Me4)Y(C5Me5)
Schmiege, Benjamin M.; Fieser, Megan E.; Ziller, Joseph W.; Evans, William J.; Organometallics 31 (2012) 5591–; doi:10.1021/om300546t

data_4078938
_publ_section_title
;
 Reactivity of the Y3+Tuck-Over Hydride Complex,
 (C5Me5)2Y(\m-H)(\m-CH2C5Me4)Y(C5Me5)
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5591
_journal_paper_doi               10.1021/om300546t
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C46 H65 Cl Y2'
_chemical_formula_weight         831.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 116.0716(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2433(6)
_cell_length_b                   16.9361(6)
_cell_length_c                   14.1667(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.66
_cell_volume                     4147.2(2)
_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      98(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24814
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    2.879
_exptl_absorpt_correction_T_max  0.4689
_exptl_absorpt_correction_T_min  0.4323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9849
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0367P)^2^+1.5956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                9217
_reflns_number_total             9849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300546t_si_002.cif
_cod_data_source_block           bms12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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_original_sg_symbol_H-M      C2
_cod_database_code               4078938