C-H Bonds Are Not Elongated by Coordination to Lanthanide Metals: Single-Crystal Neutron Diffraction Structures of (C5Me5)Y(OC6H3tBu2)CH(SiMe3)2 at 20 K and (C5Me5)La{CH(SiMe3)2}2 at 15 K
Wim T. Klooster; Lee Brammer; Colin J. Schaverien; Peter H. M. Budzelaar; Journal of the American Chemical Society 121 (1999) 1381–1382; doi:10.1021/ja983068b

data_4116303
_publ_section_title
;
 C-H Bonds Are Not Elongated by Coordination to Lanthanide Metals:
 Single-Crystal Neutron Diffraction Structures of
 (C5Me5)Y(OC6H3tBu2)CH(SiMe3)2 at 20 K and (C5Me5)La{CH(SiMe3)2}2 at 15 K
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1381
_journal_page_last               1382
_journal_paper_doi               10.1021/ja983068b
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_sum            'C31 H55 O Si2 Y'
_chemical_formula_weight         588.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.476(3)
_cell_length_b                   22.133(8)
_cell_length_c                   15.815(5)
_cell_measurement_temperature    128(5)
_cell_volume                     3315.4(19)
_computing_cell_refinement       'P3 (siemens, 1991)'
_computing_data_collection       'P3 (Siemens, 1991)'
_computing_data_reduction        'XDISK (Siemens, 1991)'
_computing_molecular_graphics    'SHELXTL 5.0 (Siemens, 1994)'
_computing_publication_material  'SHELXTL 5.0 (Siemens, 1994)'
_computing_structure_refinement  'SHELXTL 5.0 (Siemens, 1994)'
_computing_structure_solution    'SHELXTL 5.0 (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V diffractometer'
_diffrn_measurement_method       'w/2q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.1230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6104
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.851
_exptl_absorpt_correction_T_max  0.427
_exptl_absorpt_correction_T_min  0.539
_exptl_absorpt_correction_type   'semi-empirical (SHELXTL 5.0)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_F_000             1264
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.993
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_obs          0.0695
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2285
_refine_ls_wR_factor_obs         0.1548
_reflns_number_observed          3549
_reflns_number_total             5740
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja983068b_1.cif
_cod_data_source_block           l3592abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116303