#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/96/2009654.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009654
loop_
_publ_author_name
'Müller, Ulrich'
'Sens, Irina'
'Wollert, René'
'Dehnicke, Kurt'
_publ_section_title
;
 [Me₃PhN]₂[WCl₆] und
 [PPh₄]₂[W₂Cl₆O₂(μ-N)(μ-Cl₂PO₂)], ein
 μ-N-Nitridowolframat mit Dichlorophosphatbrücke
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              493
_journal_page_last               496
_journal_paper_doi               10.1107/S0108270193010753
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C48 H40 Cl8 N O4 P3 W2'
_chemical_formula_weight         1439.1
_chemical_name_common
; Tetraphenylphosphophonium hexachlorodioxo-μ-dichlorophospato-μ-nitrido-
ditungstide
;
_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'
_cell_angle_alpha                90.0
_cell_angle_beta                 115.36(4)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   27.369(7)
_cell_length_b                   11.349(2)
_cell_length_c                   18.451(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      16
_cell_measurement_theta_min      7
_cell_volume                     5179(3)
_computing_cell_refinement       'CAD-4 Meßsoftware'
_computing_data_collection       'CAD-4 Meßsoftware'
_computing_data_reduction        'XCAD-4 (Harms, 1987)'
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1989)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω/θ-scan
_diffrn_radiation_monochromator  Graphit
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4698
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.5
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.990
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   'empirisch nach \y-scans'
_exptl_crystal_colour            gr\"un
_exptl_crystal_density_diffrn    1.85
_exptl_crystal_description       'dünne Nadel'
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.24
_refine_diff_density_min         -0.97
_refine_ls_extinction_method     keine
_refine_ls_goodness_of_fit_obs   1.5
_refine_ls_hydrogen_treatment
; geometrisch berechnete Positionen angenommen, ein gemeinsamer isotroper
  Temperaturfaktor
;
_refine_ls_matrix_type           'volle Matrix'
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3454
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_obs          0.041
_refine_ls_shift/esd_max         0.23
_refine_ls_shift/esd_mean        0.08
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fₒ)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.030
_reflns_number_observed          3454
_reflns_number_total             4558
_reflns_observed_criterion       F>3\s(F)
_cod_data_source_file            se1037.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F~o~)]' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w = 1/[\s^2^(F~o~)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5178.8(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2009654
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y,1/2-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2-y,-z
1/2-x,1/2+y,1/2-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
W 0.063560(10) 0.12444(3) 0.23558(2) 0.03440(10)
Cl(1) 0.11239(8) 0.1580(3) 0.37380(10) 0.0770(10)
Cl(2) 0.01180(10) 0.1375(3) 0.09720(10) 0.0970(10)
Cl(3) 0.13661(8) 0.2072(2) 0.21650(10) 0.0600(10)
Cl(4) 0.03770(10) 0.4861(3) 0.3409(2) 0.124(2)
P(1) 0.0000 0.3766(3) 0.2500 0.0550(10)
O(1) 0.0820(2) -0.0170(5) 0.2355(3) 0.072(3)
O(2) 0.0411(2) 0.3135(4) 0.2341(3) 0.059(2)
N 0.0000 0.1045(5) 0.2500 0.010(2)
P(2) 0.17016(7) 0.3113(2) 0.82610(10) 0.0304(6)
C(11) 0.1286(3) 0.2867(6) 0.8778(3) 0.030(2)
C(12) 0.1477(3) 0.3163(7) 0.9577(4) 0.044(2)
C(13) 0.1167(3) 0.2855(7) 0.9998(4) 0.054(2)
C(14) 0.0704(3) 0.2242(8) 0.9614(5) 0.063(2)
C(15) 0.0511(3) 0.1963(8) 0.8817(5) 0.064(2)
C(16) 0.0802(3) 0.2285(7) 0.8388(4) 0.046(2)
C(21) 0.2099(3) 0.1817(6) 0.8358(3) 0.030(2)
C(22) 0.2426(3) 0.1746(6) 0.7940(4) 0.041(2)
C(23) 0.2738(3) 0.0754(7) 0.8039(4) 0.048(2)
C(24) 0.2723(3) -0.0162(7) 0.8510(4) 0.049(2)
C(25) 0.2388(3) -0.0111(7) 0.8886(4) 0.049(2)
C(26) 0.2074(3) 0.0865(6) 0.8820(4) 0.034(2)
C(31) 0.1293(3) 0.3352(6) 0.7204(4) 0.035(2)
C(32) 0.1187(3) 0.2426(7) 0.6672(4) 0.049(2)
C(33) 0.0866(3) 0.2606(8) 0.5862(5) 0.062(2)
C(34) 0.0666(3) 0.3684(8) 0.5601(5) 0.066(2)
C(35) 0.0758(3) 0.4640(7) 0.6106(5) 0.059(2)
C(36) 0.1069(3) 0.4475(7) 0.6924(4) 0.047(2)
C(41) 0.2147(3) 0.4355(6) 0.8691(4) 0.033(2)
C(42) 0.1928(3) 0.5427(7) 0.8782(4) 0.043(2)
C(43) 0.2264(3) 0.6403(7) 0.9066(4) 0.050(2)
C(44) 0.2801(3) 0.6295(8) 0.9281(4) 0.052(2)
C(45) 0.3023(3) 0.5248(7) 0.9225(4) 0.054(2)
C(46) 0.2697(3) 0.4260(7) 0.8924(4) 0.046(2)
H(12) 0.1811 0.3603 0.9844 0.063
H(13) 0.1303 0.3104 1.0555 0.063
H(14) 0.0479 0.2081 0.9905 0.063
H(15) 0.0165 0.1557 0.8544 0.063
H(16) 0.0674 0.2057 0.7833 0.063
H(22) 0.2443 0.2400 0.7630 0.063
H(23) 0.2981 0.0719 0.7772 0.063
H(24) 0.2947 -0.0871 0.8569 0.063
H(25) 0.2375 -0.0781 0.9224 0.063
H(26) 0.1837 0.0898 0.9082 0.063
H(32) 0.1331 0.1672 0.6873 0.063
H(33) 0.0794 0.1961 0.5493 0.063
H(34) 0.0433 0.3837 0.5012 0.063
H(35) 0.0609 0.5424 0.5911 0.063
H(36) 0.1146 0.5135 0.7292 0.063
H(42) 0.1541 0.5491 0.8616 0.063
H(43) 0.2100 0.7157 0.9106 0.063
H(44) 0.3035 0.7005 0.9482 0.063
H(45) 0.3412 0.5188 0.9367 0.063
H(46) 0.2853 0.3522 0.8878 0.063
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl(1) W Cl(2) 1 1 1 166.90(10) yes
Cl(1) W Cl(3) 1 1 1 88.40(10) yes
Cl(1) W O(1) 1 1 1 97.2(2) yes
Cl(1) W O(2) 1 1 1 83.3(2) yes
Cl(1) W N 1 1 1 89.80(10) yes
Cl(2) W Cl(3) 1 1 1 88.20(10) yes
Cl(2) W O(1) 1 1 1 95.8(2) yes
Cl(2) W O(2) 1 1 1 83.7(2) yes
Cl(2) W N 1 1 1 89.90(10) yes
Cl(3) W O(1) 1 1 1 96.0(2) yes
Cl(3) W O(2) 1 1 1 82.1(2) yes
Cl(3) W N 1 1 1 163.5(2) yes
O(1) W O(2) 1 1 1 178.1(3) yes
O(1) W N 1 1 1 100.4(3) yes
O(2) W N 1 1 1 81.4(2) yes
Cl(4) P(1) O(2) 1 1 1 108.0(2) yes
Cl(4) P(1) Cl(4) 1 1 3 102.5(2) yes
Cl(4) P(1) O(2) 1 1 3 107.6(2) yes
O(2) P(1) O(2) 1 1 3 121.5(4) yes
W(1) O(2) P(1) 1 1 3 134.4(4) yes
W N W 1 1 3 166.2(3) yes
C(11) P(2) C(21) 1 1 1 108.4(3) yes
C(11) P(2) C(31) 1 1 1 110.9(3) yes
C(11) P(2) C(41) 1 1 1 110.5(3) yes
C(21) P(2) C(31) 1 1 1 107.5(3) yes
C(21) P(2) C(41) 1 1 1 109.3(3) yes
C(31) P(2) C(41) 1 1 1 110.3(3) yes
P(2) C(11) C(12) 1 1 1 119.6(6) no
P(2) C(11) C(16) 1 1 1 119.0(5) no
C(12) C(11) C(16) 1 1 1 121.1(7) no
C(11) C(12) C(13) 1 1 1 118.9(7) no
C(12) C(13) C(14) 1 1 1 119.2(7) no
C(13) C(14) C(15) 1 1 1 121.6(9) no
C(14) C(15) C(16) 1 1 1 120.0(9) no
C(11) C(16) C(15) 1 1 1 119.1(7) no
P(2) C(21) C(22) 1 1 1 119.5(5) no
P(2) C(21) C(26) 1 1 1 120.7(6) no
C(22) C(21) C(26) 1 1 1 119.8(6) no
C(21) C(22) C(23) 1 1 1 118.4(7) no
C(22) C(23) C(24) 1 1 1 121.4(8) no
C(23) C(24) C(25) 1 1 1 119.9(8) no
C(24) C(25) C(26) 1 1 1 121.2(7) no
C(21) C(26) C(25) 1 1 1 119.1(7) no
P(2) C(31) C(32) 1 1 1 119.8(5) no
P(2) C(31) C(36) 1 1 1 120.2(5) no
C(32) C(31) C(36) 1 1 1 119.9(6) no
C(31) C(32) C(33) 1 1 1 119.8(7) no
C(32) C(33) C(34) 1 1 1 119.6(8) no
C(33) C(34) C(35) 1 1 1 123.1(7) no
C(34) C(35) C(36) 1 1 1 118.3(8) no
C(31) C(36) C(35) 1 1 1 119.2(7) no
P(2) C(41) C(42) 1 1 1 119.1(6) no
P(2) C(41) C(46) 1 1 1 121.0(6) no
C(42) C(41) C(46) 1 1 1 119.8(7) no
C(41) C(42) C(43) 1 1 1 119.3(8) no
C(42) C(43) C(44) 1 1 1 119.8(8) no
C(43) C(44) C(45) 1 1 1 121.5(8) no
C(44) C(45) C(46) 1 1 1 120.2(8) no
C(41) C(46) C(45) 1 1 1 119.2(7) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W Cl(1) 1 1 2.348(2) yes
W Cl(2) 1 1 2.334(2) yes
W Cl(3) 1 1 2.367(3) yes
W O(1) 1 1 1.683(5) yes
W O(2) 1 1 2.229(5) yes
W N 1 1 1.8830(10) yes
P(1) Cl(4) 1 1 1.985(4) yes
P(1) O(2) 1 1 1.465(6) yes
P(2) C(11) 1 1 1.793(8) yes
P(2) C(21) 1 1 1.791(7) yes
P(2) C(31) 1 1 1.804(7) yes
P(2) C(41) 1 1 1.810(7) yes
C(11) C(12) 1 1 1.380(10) no
C(11) C(16) 1 1 1.370(10) no
C(12) C(13) 1 1 1.420(10) no
C(13) C(14) 1 1 1.350(10) no
C(14) C(15) 1 1 1.370(10) no
C(15) C(16) 1 1 1.390(10) no
C(21) C(22) 1 1 1.410(10) no
C(21) C(26) 1 1 1.400(10) no
C(22) C(23) 1 1 1.380(10) no
C(23) C(24) 1 1 1.370(10) no
C(24) C(25) 1 1 1.370(10) no
C(25) C(26) 1 1 1.370(10) no
C(31) C(32) 1 1 1.380(10) no
C(31) C(36) 1 1 1.410(10) no
C(32) C(33) 1 1 1.390(10) no
C(33) C(34) 1 1 1.340(10) no
C(34) C(35) 1 1 1.380(10) no
C(35) C(36) 1 1 1.390(10) no
C(41) C(42) 1 1 1.400(10) no
C(41) C(46) 1 1 1.380(10) no
C(42) C(43) 1 1 1.390(10) no
C(43) C(44) 1 1 1.350(10) no
C(44) C(45) 1 1 1.360(10) no
C(45) C(46) 1 1 1.390(10) no
