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_4324050
_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            'C16 H17 F5 N O2.5 W'
_chemical_formula_weight         542.16
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.246(3)
_cell_length_b                   10.043(2)
_cell_length_c                   14.102(3)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1817.3(7)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'Siemens SHELXTL-Plus'
_computing_publication_material  'SHELXTL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device
'Stoe-Siemens-AED2 four-circle-diffractometer'
_diffrn_measurement_method       'Profile data from 2theta/omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3977
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         4.06
_diffrn_standards_decay_%        15
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.417
_exptl_absorpt_correction_T_max  0.9690
_exptl_absorpt_correction_T_min  0.4015
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.227
_refine_diff_density_rms         .119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2345
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.019
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_obs          0.0295
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0469P)^2^+4.0294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0765
_refine_ls_wR_factor_obs         0.0735
_reflns_number_observed          2221
_reflns_number_total             2349
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950919x_1.cif
_cod_data_source_block           hallo2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0469P)^2^+4.0294P] 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^)+( 0.0469P)^2^+4.0294P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1817.3(6)
_cod_original_formula_sum        'C16 H17 F5 N O2.50 W'
_cod_database_code               4324050