Syntheses, Structures, and Reactivity of a Series of (Pentamethylcyclopentadienyl)molybdenum(V) and -tungsten(V) Imido Complexes
Katrin Köhler; Herbert W. Roesky; Axel Herzog; Heinz Gornitzka; Alexander Steiner; Isabel Usón; Inorganic Chemistry 35 (1996) 1773–1777; doi:10.1021/ic950919x

data_4324052
_publ_section_title
;
 Syntheses, Structures, and Reactivity of a Series of
 (Pentamethylcyclopentadienyl)molybdenum(V) and -tungsten(V) Imido
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1773
_journal_page_last               1777
_journal_paper_doi               10.1021/ic950919x
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C14 H24 Cl2 Mo N'
_chemical_formula_weight         373.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6040(10)
_cell_length_b                   12.0490(10)
_cell_length_c                   17.020(2)
_cell_measurement_temperature    223(2)
_cell_volume                     1764.5(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8121
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    1.032
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.055
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_restrained_S_obs      1.055
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_obs          0.0213
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.7687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0570
_refine_ls_wR_factor_obs         0.0561
_reflns_number_observed          2269
_reflns_number_total             2294
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950919x_3.cif
_cod_data_source_block           roe437
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.7687P] 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^)+(0.0312P)^2^+0.7687P] 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               4324052