Tungsten Allylimido Complexes Cl4(RCN)W(NC3H5) as Single-Source CVD Precursors for WNxCyThin Films. Correlation of Precursor Fragmentation to Film Properties
Omar J. Bchir; Kelly M. Green; Hiral M. Ajmera; Elizabeth A. Zapp; Timothy J. Anderson; Benjamin C. Brooks; Laurel L. Reitfort; David H. Powell; Khalil A. Abboud; Lisa McElwee-White; Journal of the American Chemical Society 127 (2005) 7825–7833; doi:10.1021/ja043799d

data_4111717
_publ_section_title
;
 Tungsten Allylimido Complexes Cl4(RCN)W(NC3H5) as Single-Source CVD
 Precursors for WNxCyThin Films. Correlation of Precursor Fragmentation to
 Film Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7825
_journal_page_last               7833
_journal_paper_doi               10.1021/ja043799d
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C5 H8 Cl4 N2 W'
_chemical_formula_weight         421.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.089(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1482(7)
_cell_length_b                   7.4742(8)
_cell_length_c                   12.3697(13)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     566.18(11)
_computing_cell_refinement       'Bruker SMART & SAINT (Bruker 1998)'
_computing_data_collection       'Bruker SMART (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3692
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.097
_exptl_absorpt_correction_T_max  0.6624
_exptl_absorpt_correction_T_min  0.3050
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, SHELXTL (Bruker 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_meas      0
_exptl_crystal_description       plates
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.818
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0478P)^2^+1.6766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                1939
_reflns_number_total             2287
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja043799dsi20041025_014843.cif
_cod_data_source_block           lr01
_cod_database_code               4111717