An N-bridged tritungsten compound for the chemical vapor deposition of WN~<i>x~</i> thin films
Koller, Jürgen; McElwee-White, Lisa; Abboud, Khalil A.; Acta Crystallographica Section E 63 (2007) m2733–m2733; doi:10.1107/S1600536807049033

data_2216183
_publ_section_title
;
 An N-bridged tritungsten compound for the chemical vapor deposition of
 WN~<i>x~</i> thin films
;
_journal_coeditor_code           ZL2070
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2733
_journal_page_last               m2733
_journal_paper_doi               10.1107/S1600536807049033
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac
'[W3 (C3 H9 N Si)2 Cl8 N2 (C5 H5 N)4], 2C H2 Cl2'
_chemical_formula_moiety         'C26 H38 Cl8 N8 Si2 W3, 2(C H2 Cl2)'
_chemical_formula_sum            'C28 H42 Cl12 N8 Si2 W3'
_chemical_formula_weight         1523.83
_chemical_name_systematic
;
octachlorido-1\k^4^Cl,3\k^4^Cl-di-\m~2~-nitrido-1:2\k^2^N:N;2:3\k^2^N:N-\
tetrapyridine-1\kN,2\k^2^N,3\kN-bis(trimethylsilylimido-2\kN)tritungsten(V)
dichloromethane disolvate
;
_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                 94.329(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0546(8)
_cell_length_b                   19.5493(15)
_cell_length_c                   25.359(2)
_cell_measurement_reflns_used    4105
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     4970.4(7)
_computing_cell_refinement       'SAINT (Bruker 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SHELXTL (Sheldrick, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15825
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.650
_exptl_absorpt_correction_T_max  0.7363
_exptl_absorpt_correction_T_min  0.1071
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'[based on measured indexed crystal faces (SHELXTL; Sheldrick, 2000)]'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.758
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.758
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0063P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                3802
_reflns_number_total             5688
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2070.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4970.3(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2216183
_cod_database_fobs_code          2216183