Neutron Diffraction Studies on a 4-Coordinate Hydrogen Atom in an Yttrium Cluster
Muhammed Yousufuddin; Matthias J. Gutmann; Jens Baldamus; Olivier Tardif; Zhaomin Hou; Sax A. Mason; Garry J. McIntyre; Robert Bau; Journal of the American Chemical Society 130 (2008) 3888–3891; doi:10.1021/ja076520c

data_4107578
_publ_contact_author_address
;University of Southern California
Department of Chemistry
3620 McClintock Ave
SGM 418
Los Angeles, CA 90089
;
_publ_contact_author_email       bau@usc.edu
_publ_contact_author_name        'Robert Bau'
_publ_contact_author_phone       213-740-2692
_publ_section_title
;
 Neutron Diffraction Studies on a 4-Coordinate Hydrogen Atom in an Yttrium
 Cluster
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3888
_journal_page_last               3891
_journal_paper_doi               10.1021/ja076520c
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         Y4H8(C5Me4(SiMe3)4(THF)
_chemical_formula_sum            'C52 H100 O Si4 Y4'
_chemical_formula_weight         1209.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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-97
_cell_angle_alpha                80.443(11)
_cell_angle_beta                 86.673(10)
_cell_angle_gamma                74.379(10)
_cell_formula_units_Z            2
_cell_length_a                   12.988(2)
_cell_length_b                   13.134(2)
_cell_length_c                   19.626(3)
_cell_measurement_reflns_used    330
_cell_measurement_temperature    100(2)
_cell_volume                     3179.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.029
_diffrn_measured_fraction_theta_max 0.029
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.37-8.8A
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11132
_diffrn_reflns_theta_full        83.83
_diffrn_source                   'ISIS spallation source'
_diffrn_source_type              SXD
_exptl_absorpt_coefficient_mu    '5.3538 + 0.01369 * lambda'
_exptl_absorpt_correction_T_max  2.1934
_exptl_absorpt_correction_T_min  1.9784
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'gaussian integration with 32 grid points'
_exptl_crystal_colour            yellow
_exptl_crystal_description       prism
_exptl_crystal_recrystallization_method 'Hexane at -30 C'
_refine_diff_density_max         1.896
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.00101(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1434
_refine_ls_number_reflns         11132
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.993
_refine_ls_shift/su_mean         0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1825P)^2^+58.8393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2240
_refine_ls_wR_factor_ref         0.2240
_reflns_number_gt                11132
_reflns_number_total             11132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076520c-file003.cif
_cod_data_source_block           final_isis_dfix
_cod_original_cell_volume        3179.3(9)
_cod_database_code               4107578