Structural Reassessment of [W(CO)5(TCNE)]: N (σ) Coordination Instead of an Olefin (π) Complex
Bubrin, Martina; Krafft, Michael J.; Steudle, Lisa; Hübner, Ralph; Field, John S.; Záliš, Stanislav; Kaim, Wolfgang; Organometallics 31 (2012) 6305–; doi:10.1021/om300565q

data_4079200
_publ_section_title
;
 Structural Reassessment of [W(CO)5(TCNE)]: N (\s) Coordination Instead of
 an Olefin (\p) Complex
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6305
_journal_paper_doi               10.1021/om300565q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C11 N4 O5 W, 0.5(C6 N4)'
_chemical_formula_sum            'C14 N6 O5 W'
_chemical_formula_weight         516.05
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.495(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.6938(18)
_cell_length_b                   9.3704(7)
_cell_length_c                   7.3889(5)
_cell_measurement_reflns_used    3336
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.72
_cell_volume                     1639.9(2)
_computing_cell_refinement       'Bruker APEX II Software Suite, 2008'
_computing_data_collection       'Bruker APEX II Software Suite, 2008'
_computing_data_reduction        'Bruker APEX II Software Suite, 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'Omega + Phi 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  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20785
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.084
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.966
_refine_diff_density_min         -8.916
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+93.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                1968
_reflns_number_total             3336
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300565q_si_002.cif
_cod_data_source_block           ac54x
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4079200