Silylene Hydride Complexes of Molybdenum with Silicon-Hydrogen Interactions: Neutron Structure of (η5-C5Me5)(Me2PCH2CH2PMe2)Mo(H)(SiEt2)
Benjamin V. Mork; T. Don Tilley; Arthur J. Schultz; John A. Cowan; Journal of the American Chemical Society 126 (2004) 10428–10440; doi:10.1021/ja040026g

data_4112870
_publ_section_title
;
 Silylene Hydride Complexes of Molybdenum with Silicon-Hydrogen
 Interactions: Neutron Structure of
 (\h5-C5Me5)(Me2PCH2CH2PMe2)Mo(H)(SiEt2)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10428
_journal_page_last               10440
_journal_paper_doi               10.1021/ja040026g
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C123 H48 Mo P2 Si2'
_chemical_formula_weight         538.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.229(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0505(5)
_cell_length_b                   14.5815(8)
_cell_length_c                   21.9795(12)
_cell_measurement_reflns_used    4472
_cell_measurement_temperature    128(1)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      4
_cell_volume                     2883.5(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      128(1)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       '\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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12724
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.964
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1117
_refine_ls_wR_factor_obs         0.1004
_reflns_number_observed          3379
_reflns_number_total             4861
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja040026g_6.cif
_cod_data_source_block           compound_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0656P)^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^)+(0.0656P)^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               4112870