Cyclopentadienylmolybdenum(II) and -(III) Complexes Containing Diene and Allyl Ligands. 1. Isomeric Preferences and Isomerization Rates in a Pair of Redox-Related Organometallic Complexes
Li-Sheng Wang; James C. Fettinger; Rinaldo Poli; Journal of the American Chemical Society 119 (1997) 4453–4464; doi:10.1021/ja964078k

data_4116974
_publ_section_title
;
 Cyclopentadienylmolybdenum(II) and -(III) Complexes Containing Diene and
 Allyl Ligands. 1. Isomeric Preferences and Isomerization Rates in a Pair
 of Redox-Related Organometallic Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4453
_journal_page_last               4464
_journal_paper_doi               10.1021/ja964078k
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C12 H16 Mo'
_chemical_formula_weight         256.19
_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                 111.927(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4437(5)
_cell_length_b                   7.3498(4)
_cell_length_c                   12.0043(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      17.9
_cell_volume                     1018.48(8)
_computing_cell_refinement       'Enraf EXPRESS'
_computing_data_collection       'Enraf EXPRESS'
_computing_data_reduction        'XCAD4 (Harms, 1993); Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'omega-2theta 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  0.0067
_diffrn_reflns_av_sigmaI/netI    0.0097
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1888
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         3.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  0.7363
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brownish-orange
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0027(3)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         1793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_obs          0.0163
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.3997P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0438
_refine_ls_wR_factor_obs         0.0410
_reflns_number_observed          1510
_reflns_number_total             1793
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja964078k_2.cif
_cod_data_source_block           compound_4a
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.3997P] where P=3D(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=3D1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.3997P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116974