W2Cl4(NHR)2(PR'3)2 Molecules. 3. Bidentate Phosphine Complexes of Bis(tert-butylamido)tetrachloroditungsten. Preparation and Structural Characterization of cis,cis-W2Cl4(NHCMe3)2(L-L) (L-L = dmpm, dmpe, dppm, dppe)
F. Albert Cotton; Evgeny V. Dikarev; Wai-Yeung Wong; Inorganic Chemistry 36 (1997) 80–85; doi:10.1021/ic960906z

data_4323274
_publ_section_title
;
 W2Cl4(NHR)2(PR'3)2 Molecules. 3. Bidentate Phosphine Complexes of
 Bis(tert-butylamido)tetrachloroditungsten. Preparation and Structural
 Characterization of cis,cis-W2Cl4(NHCMe3)2(L-L) (L-L = dmpm, dmpe, dppm,
 dppe)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              80
_journal_page_last               85
_journal_paper_doi               10.1021/ic960906z
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C14 H36 Cl4 N2 P2 W2'
_chemical_formula_structural     W2Cl4(NHCMe3)2(DMPE)
_chemical_formula_sum            'C14 H36 Cl4 N2 P2 W2'
_chemical_formula_weight         803.89
_chemical_melting_point          ?
_chemical_name_common
; 
 cis-Tetrachloro-bis(t-butylamido)-dimethylphosphinoethan
 ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(t-butylamido)-(cis)-1,2-
 dimethylphosphinoethan ditungsten(III) 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.50(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.144(2)
_cell_length_b                   11.991(1)
_cell_length_c                   15.662(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34
_cell_measurement_theta_min      23
_cell_volume                     2503.9(5)
_computing_cell_refinement       'TEXSAN-TEXRAY (1985)'
_computing_data_collection       'TEXSAN-TEXRAY (1985)'
_computing_data_reduction        'TEXSAN-TEXRAY (1985)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3897
_diffrn_reflns_theta_max         60.07
_diffrn_reflns_theta_min         3.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    21.877
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4952
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.240
_refine_diff_density_min         -1.821
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00050(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL-93
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_obs          0.0343
_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^)+(0.0312P)^2^+21.8118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0950
_refine_ls_wR_factor_obs         0.0878
_reflns_number_observed          3316
_reflns_number_total             3727
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic960906z_3.cif
_cod_data_source_block           W2Cl4(NHCMe3)2(DMPE)
_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^)+(0.0312P)^2^+21.8118P] 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^)+(0.0312P)^2^+21.8118P] 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               4323274