New Tungsten(VI) Guanidinato Complexes: Synthesis, Characterization, and Application in Metal−Organic Chemical Vapor Deposition of Tungsten Nitride Thin Films
Rische, Daniel; Parala, Harish; Gemel, Eliza; Winter, Manuela; Fischer, Roland A.; Chemistry of Materials 18 (2006) 6075–; doi:10.1021/cm061999d

data_4001600
_publ_section_title
;
 New Tungsten(VI) Guanidinato Complexes:&#x00A0; Synthesis,
 Characterization, and Application in Metal&#x2212;Organic Chemical Vapor
 Deposition of Tungsten Nitride Thin Films
;
_journal_issue                   25
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6075
_journal_paper_doi               10.1021/cm061999d
_journal_volume                  18
_journal_year                    2006
_chemical_formula_sum            'C17 H38 Cl N5 W'
_chemical_formula_weight         531.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 103.140(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.399(2)
_cell_length_b                   9.5815(15)
_cell_length_c                   32.617(5)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.80
_cell_volume                     4686.5(12)
_computing_cell_refinement       'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 1.171.13, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '1258 images at 1.0 deg. in \w and 20 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1318
_diffrn_reflns_av_sigmaI/netI    0.2176
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            25882
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    5.052
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2127
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.900
_refine_diff_density_min         -2.424
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.849
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                2734
_reflns_number_total             5333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm061999dsi20060824_091720.cif
_cod_data_source_block           cc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4001600