[Me~3~PhN]~2~[WCl~6~] und [PPh~4~]~2~[W~2~Cl~6~O~2~(μ-N)(μ-Cl~2~PO~2~)], ein μ-<i>N</i>-Nitridowolframat mit Dichlorophosphatbrücke
Müller, Ulrich; Sens, Irina; Wollert, René; Dehnicke, Kurt; Acta Crystallographica Section C 50 (1994) 493–496; doi:10.1107/S0108270193010753

data_2009654
_publ_section_title
;
 [Me~3~PhN]~2~[WCl~6~] und
 [PPh~4~]~2~[W~2~Cl~6~O~2~(\m-N)(\m-Cl~2~PO~2~)], ein
 \m-<i>N</i>-Nitridowolframat mit Dichlorophosphatbr\"ucke
;
_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-\m-dichlorophospato-\m-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 Me\&ssoftware'
_computing_data_collection       'CAD-4 Me\&ssoftware'
_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       \w/\q-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       'd\"unne 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/[\s^2^(F~o~)]'
_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