Synthesis, Crystal Structures, and Fluxional Behavior of Donor-Bridged Bis(silylene)molybdenum and -chromium Complexes
Ueno, Keiji; Masuko, Akira; Ogino, Hiroshi; Organometallics 18 (1999) 2694–; doi:10.1021/om990201f

data_4077789
_publ_section_title
;
 Synthesis, Crystal Structures, and Fluxional Behavior of Donor-Bridged
 Bis(silylene)molybdenum and -chromium Complexes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2694
_journal_paper_doi               10.1021/om990201f
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C12 H20 Mo O3 Si2'
_chemical_formula_weight         364.40
_chemical_name_systematic
;
 ?
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.89(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0938(13)
_cell_length_b                   12.0680(9)
_cell_length_c                   9.0823(7)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.99
_cell_measurement_theta_min      12.59
_cell_volume                     1645.6(2)
_computing_cell_refinement       urlap
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        f2-lp
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-\2q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4786
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        10.2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.079
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_obs          0.0356
_refine_ls_shift/esd_max         -0.117
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.3492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0940
_refine_ls_wR_factor_obs         0.0835
_reflns_number_observed          3621
_reflns_number_total             4786
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om990201f.cif
_cod_data_source_block
;
;
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.3492P] 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^)+(0.0441P)^2^+0.3492P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4077789