W2Cl4(NR2)2(PR'3)2 Molecules. 4. A New Synthetic Route to Products with a Staggered Conformation. Preparations and Characterizations of W2Cl4(NR2)2(PR'3)2 (R = Et, Bu, Hex; R'3= Me3, Et2H) and an Intermediate Complex W2Cl4(NEt2)2(NHEt2)2
F. Albert Cotton; Evgeny V. Dikarev; N. Nawar; Wai-Yeung Wong; Inorganic Chemistry 36 (1997) 559–566; doi:10.1021/ic9610694

data_4323319
_publ_section_title
;
 W2Cl4(NR2)2(PR'3)2 Molecules. 4. A New Synthetic Route to Products with a
 Staggered Conformation. Preparations and Characterizations of
 W2Cl4(NR2)2(PR'3)2 (R = Et, Bu, Hex; R'3= Me3, Et2H) and an Intermediate
 Complex W2Cl4(NEt2)2(NHEt2)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              559
_journal_page_last               566
_journal_paper_doi               10.1021/ic9610694
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C22 H54 Cl4 N2 P2 W2'
_chemical_formula_structural     W2Cl4(NBu2)2(PMe3)2
_chemical_formula_sum            'C22 H54 Cl4 N2 P2 W2'
_chemical_formula_weight         918.11
_chemical_melting_point          ?
_chemical_name_common
;
 cis,cis-Tetrachloro-bis(dibutylamido)-bis(trimethyl-
 phosphine) ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(dibutylamido)-(cis,cis)-
 1,2-bis(trimethylphosphine) ditungsten(III) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.66(3)
_cell_angle_beta                 97.99(4)
_cell_angle_gamma                91.26(3)
_cell_formula_units_Z            4
_cell_length_a                   12.162(6)
_cell_length_b                   14.955(4)
_cell_length_c                   18.82(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      14.33
_cell_measurement_theta_min      11.26
_cell_volume                     3371(3)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V5 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9879
_diffrn_reflns_theta_max         22.95
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.244
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.3085
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.526
_refine_diff_density_min         -3.266
_refine_diff_density_rms         0.327
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.039
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_obs          0.0576
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1194P)^2^+12.5977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1709
_refine_ls_wR_factor_obs         0.1473
_reflns_number_observed          7435
_reflns_number_total             9357
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic9610694_4.cif
_cod_data_source_block           W2Cl4(NBu2)2(PMe3)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1194P)^2^+12.5977P] 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^)+(0.1194P)^2^+12.5977P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323319