Synthesis, Structure, and Electrochemistry of Fischer Alkoxy- and Aminocarbene Complexes of Tungsten: The Use of DFT To Predict and Understand Oxidation and Reduction Potentials
Landman, Marilé; Pretorius, René; Buitendach, Blenerhassitt E.; van Rooyen, Petrus H.; Conradie, Jeanet; Organometallics 32 (2013) 5491–; doi:10.1021/om400778z

data_4089612
_publ_section_title
;
 Synthesis, Structure, and Electrochemistry of Fischer Alkoxy- and
 Aminocarbene Complexes of Tungsten: The Use of DFT To Predict and
 Understand Oxidation and Reduction Potentials
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5491
_journal_paper_doi               10.1021/om400778z
_journal_volume                  32
_journal_year                    2013
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_space_group_name_Hall           'A 2 -2a'
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_atom_sites_solution_primary     'intrinsic phasing'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6044(9)
_cell_length_b                   12.0731(7)
_cell_length_c                   14.8012(5)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.61
_cell_measurement_theta_min      3.15
_cell_volume                     1358.88(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
; <i>ORTEP-3 for Windows</i> (Farrugia, 1997),
 <i>Mercury</i> (Macrae <i>et al</i>., 2008)
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;
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_radiation_source         'I\ms micro focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            103124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         52.585
_diffrn_reflns_theta_min         2.177
_exptl_absorpt_coefficient_mu    8.528
_exptl_absorpt_correction_T_max  0.7504
_exptl_absorpt_correction_T_min  0.3277
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_exptl_absorpt_process_details   SADABS
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_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details
;
 Flack x determined using 3605 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.482(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         8269
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.194
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+2.8676P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7728
_reflns_number_total             8269
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           compound_2
_cod_database_code               4089612
_shelxl_version_number           2013-2
_shelx_res_checksum              64393
_shelx_hkl_checksum              70708