Oxidation of the zwitterionic tungsten amide (OC)5WNPhNPhC(OMe)Ph with Br2 and PCl5. Formation of [(PhN)W(CO)2X2]2 and (PhN)W(CO)2X2L (X = Br or Cl; L = MeCN, Me3C6H2NH2 and i-BuNH2)
He, Yingxia; McGowan, Patrick C.; Abboud, Khalil A.; McElwee-White, Lisa; Journal of the Chemical Society, Dalton Transactions  (1998) 3373–; doi:10.1039/a803989e

data_7028045
_publ_section_title
;
 Oxidation of the zwitterionic tungsten amide (OC)5WNPhNPhC(OMe)Ph with
 Br2 and PCl5. Formation of [(PhN)W(CO)2X2]2 and (PhN)W(CO)2X2L
 (X&#x2005;=&#x2005;Br or Cl; L&#x2005;=&#x2005;MeCN, Me3C6H2NH2 and
 i-BuNH2)
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3373
_journal_paper_doi               10.1039/a803989e
_journal_year                    1998
_chemical_formula_sum            'C16 H10 Br4 N2 O4 W2'
_chemical_formula_weight         981.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.0790(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1118(1)
_cell_length_b                   10.492
_cell_length_c                   15.7374(1)
_cell_measurement_reflns_used    5919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.34
_cell_volume                     1169.667(18)
_computing_cell_refinement       'Siemens SMART & SAINT, (Siemens, 1995)'
_computing_data_collection       'Siemens SMART, (Siemens, 1995)'
_computing_data_reduction        'Siemens SHELXTL5, (Sheldrick, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL5'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    'SHELXL-97, (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7674
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    16.682
_exptl_absorpt_correction_T_max  0.1457
_exptl_absorpt_correction_T_min  0.0590
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.674
_refine_diff_density_min         -1.898
_refine_diff_density_rms         0.285
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL-97
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+32.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                2423
_reflns_number_total             2685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            e803989sup1.cif
_cod_data_source_block           9
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+32.2400P] where P=(Fo^2^+2Fc^2^)/3'
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^(Fo^2^)+(0.0329P)^2^+32.2400P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1169.66(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7028045