#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:20:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179323 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/20/4322008.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4322008
loop_
_publ_author_name
'Hiroshige Ishino'
'Shin'ichi Tokunaga'
'Hidetake Seino'
'Youichi Ishii'
'Masanobu Hidai'
_publ_contact_author
;
    Masanobu Hidai
 Department of Chemistry and Biotechnology, Graduate School of Engineering,
The University of Tokyo, Hongo, Bunkyo-ku, Tokyo 113-8656, Japan
;
_publ_contact_author_fax         ' +81-3-5800-6945 '
_publ_contact_author_phone       ' +81-3-5800-6945 ext 7261 '
_publ_section_title
;
 Synthesis and Structures of Tungsten (1-Pyridinio)imido Complexes and
 Their Facile N-N Bond Cleavage1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2489
_journal_page_last               2496
_journal_paper_doi               10.1021/ic981116n
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C17 H23 Cl2 N O P2 W'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Mon Aug 17 14:38:10 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 110.755(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   13.0529(8)
_cell_length_b                   9.985(2)
_cell_length_c                   18.070(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      39.81
_cell_measurement_theta_min      38.66
_cell_volume                     2202.3(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.03487
_diffrn_orient_matrix_UB_12      0.00455
_diffrn_orient_matrix_UB_13      -0.05894
_diffrn_orient_matrix_UB_21      -0.07410
_diffrn_orient_matrix_UB_22      -0.00523
_diffrn_orient_matrix_UB_23      0.00446
_diffrn_orient_matrix_UB_31      -0.00229
_diffrn_orient_matrix_UB_32      0.09991
_diffrn_orient_matrix_UB_33      0.00292
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  1.63
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5564
_diffrn_reflns_theta_max         27.5215
_diffrn_standards_decay_%        -0.90
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu_cm 56.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1112.00
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         -0.68520
_refine_diff_density_min         0.45120
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.550
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3422
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0270
_refine_ls_shift/esd_max         0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0180
_cod_data_source_file            ic981116n_5.cif
_cod_data_source_block           '[WCl2(NH)(CO)(PMe2Ph)2]'
_cod_original_cell_volume        2202.2(4)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_database_code               4322008
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2-x,1/2+y,   -z'
'   -x,   -y,   -z'
'1/2+x,1/2-y,   +z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
W1 0.19712(2) 0.21264(2) -0.23294(1) 0.04538(5) Uij ? ?
Cl1 0.1256(1) 0.3585(1) -0.15184(8) 0.0681(5) Uij ? ?
Cl2 0.02413(9) 0.0780(1) -0.26793(8) 0.0634(4) Uij ? ?
P1 0.2693(1) 0.0674(1) -0.11217(7) 0.0518(4) Uij ? ?
P2 0.0979(1) 0.3625(2) -0.34748(8) 0.0640(5) Uij ? ?
O1 0.2283(3) -0.0109(4) -0.3443(2) 0.094(2) Uij ? ?
N1 0.3256(3) 0.2762(4) -0.2227(2) 0.065(1) Uij ? ?
C1 0.2179(4) 0.0699(6) -0.3031(3) 0.059(2) Uij ? ?
C2 0.1758(4) 0.0334(6) -0.0603(3) 0.086(2) Uij ? ?
C3 0.3856(4) 0.1444(5) -0.0373(3) 0.083(2) Uij ? ?
C4 0.3194(4) -0.0931(5) -0.1290(3) 0.050(2) Uij ? ?
C5 0.4033(4) -0.0983(6) -0.1595(3) 0.063(2) Uij ? ?
C6 0.4403(5) -0.2178(9) -0.1785(3) 0.086(2) Uij ? ?
C7 0.3943(7) -0.3351(7) -0.1667(4) 0.097(3) Uij ? ?
C8 0.3119(7) -0.3338(7) -0.1371(4) 0.100(3) Uij ? ?
C9 0.2748(5) -0.2128(8) -0.1182(3) 0.077(2) Uij ? ?
C10 0.1515(6) 0.5306(6) -0.3345(4) 0.125(3) Uij ? ?
C11 -0.0460(5) 0.3877(7) -0.3662(3) 0.112(3) Uij ? ?
C12 0.1056(4) 0.3068(6) -0.4409(3) 0.057(2) Uij ? ?
C13 0.0327(5) 0.2140(7) -0.4859(4) 0.100(3) Uij ? ?
C14 0.0406(7) 0.1640(9) -0.5553(5) 0.132(4) Uij ? ?
C15 0.1215(8) 0.208(1) -0.5776(5) 0.134(5) Uij ? ?
C16 0.1989(6) 0.2995(10) -0.5338(5) 0.124(4) Uij ? ?
C17 0.1887(5) 0.3473(6) -0.4646(4) 0.089(2) Uij ? ?
H1 0.3990 0.3008 -0.2367 0.0789 Uij ? ?
H2 0.1570 0.1150 -0.0413 0.0891 Uij ? ?
H3 0.1114 -0.0079 -0.0954 0.0891 Uij ? ?
H4 0.2102 -0.0248 -0.0169 0.0891 Uij ? ?
H5 0.4156 0.0838 0.0055 0.0876 Uij ? ?
H6 0.4396 0.1659 -0.0594 0.0876 Uij ? ?
H7 0.3627 0.2238 -0.0187 0.0876 Uij ? ?
H8 0.4359 -0.0171 -0.1674 0.0775 Uij ? ?
H9 0.4974 -0.2188 -0.1997 0.0980 Uij ? ?
H10 0.4199 -0.4180 -0.1792 0.1088 Uij ? ?
H11 0.2798 -0.4155 -0.1293 0.1172 Uij ? ?
H12 0.2173 -0.2127 -0.0975 0.0895 Uij ? ?
H13 0.2251 0.5293 -0.3327 0.1238 Uij ? ?
H14 0.1085 0.5847 -0.3775 0.1238 Uij ? ?
H15 0.1493 0.5664 -0.2864 0.1238 Uij ? ?
H16 -0.0555 0.4174 -0.3191 0.1149 Uij ? ?
H17 -0.0740 0.4533 -0.4065 0.1149 Uij ? ?
H18 -0.0841 0.3058 -0.3830 0.1149 Uij ? ?
H19 -0.0244 0.1831 -0.4691 0.1162 Uij ? ?
H20 -0.0107 0.1002 -0.5863 0.1487 Uij ? ?
H21 0.1265 0.1744 -0.6255 0.1543 Uij ? ?
H22 0.2566 0.3285 -0.5504 0.1402 Uij ? ?
H23 0.2408 0.4098 -0.4331 0.1063 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 68 0.003 0.002 'International Tables'
H 0 92 0.000 0.000 'International Tables'
O 0 4 0.011 0.006 'International Tables'
N 0 4 0.006 0.003 'International Tables'
W 0 4 -0.849 6.872 'International Tables'
P 0 8 0.102 0.094 'International Tables'
Cl 0 8 0.148 0.159 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 2 -2
1 1 -2
-2 1 -1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
? ? ? ? ? ?
