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_4116305
_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
;
_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_formula_structural     (C5Me5)La{CH(SiMe3)2}2
_chemical_formula_sum            'C24 H53 La Si4'
_chemical_formula_weight         592.968
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            6
_cell_length_a                   18.458(5)
_cell_length_b                   18.458(5)
_cell_length_c                   15.936(5)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    15.0(5)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     4702(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'local programs'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'SHELXTL 6.0 (Bruker, 1998)'
_computing_structure_refinement  UPALS
_computing_structure_solution    'X-ray structure coordinates'
_diffrn_ambient_temperature      15
_diffrn_measurement_device       'beamline H6S, HFBR'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  'Ge (220)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         reactor
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.15863
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5236
_diffrn_reflns_reduction_process 'local programs'
_diffrn_reflns_theta_max         54
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.2997
_exptl_absorpt_correction_T_max  0.415
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_size_max          5.3
_exptl_crystal_size_mid          5.3
_exptl_crystal_size_min          3.5
_refine_diff_density_max         '4 % of maximum'
_refine_diff_density_min         '3 % of maximum'
_refine_ls_abs_structure_details
; 
based upon X-ray structure coordinates
;
_refine_ls_extinction_coef       '0.10(1) E+04'
_refine_ls_extinction_method     'type I, isotropic'
_refine_ls_goodness_of_fit_all   1.289
_refine_ls_goodness_of_fit_obs   1.289
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         4616
_refine_ls_R_factor_all          0.221
_refine_ls_R_factor_obs          0.221
_refine_ls_shift/esd_max         0.1
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/(s^2(F^2))'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.101
_refine_ls_wR_factor_obs         0.101
_reflns_number_observed          2966
_reflns_number_total             4626
_reflns_observed_criterion       >3sigma(I)
_cod_data_source_file            ja983068b_3.cif
_cod_data_source_block           LaCpR2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/(s^2(F^2))' 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(F^2))'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4702.0(6)
_cod_original_formula_sum        'C24 H53 Si4 La1'
_cod_database_code               4116305