W2Cl4(NR2)2(PR'3)2 Molecules. 8. Synthesis and Structural Characterization of Both Cis Isomers of Stoichiometry W2Cl4(NHR)2(PMe3)2, R = Et, Prn, and Bun. Direct Evidence Favoring an Internal Flip Mechanism for Cis-Trans Isomerization
F. Albert Cotton; Evgeny V. Dikarev; Wai-Yeung Wong; Inorganic Chemistry 36 (1997) 2670–2677; doi:10.1021/ic9700361

data_4323468
_publ_section_title
;
 W2Cl4(NR2)2(PR'3)2 Molecules. 8. Synthesis and Structural
 Characterization of Both Cis Isomers of Stoichiometry W2Cl4(NHR)2(PMe3)2,
 R = Et, Prn, and Bun. Direct Evidence Favoring an Internal Flip Mechanism
 for Cis-Trans Isomerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2670
_journal_page_last               2677
_journal_paper_doi               10.1021/ic9700361
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C12 H34 Cl4 N2 P2 W2'
_chemical_formula_structural     W2Cl4(n-PrNH)2(PMe3)2
_chemical_formula_sum            'C12 H34 Cl4 N2 P2 W2'
_chemical_formula_weight         777.85
_chemical_melting_point          ?
_chemical_name_common
;
 cis,cis-Tetrachloro-bis(n-propylamido)-
 bis(trimethylphosphine) ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(n-propylamido)-(cis,cis)-
 1,2-bis(trimethylphosphine)ditungsten(III) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 92.872(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1268(8)
_cell_length_b                   10.871(1)
_cell_length_c                   17.106(1)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.80
_cell_measurement_theta_min      9.05
_cell_volume                     2438.0(3)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        MADNES
_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      213(2)
_diffrn_measurement_device       'Enraf-Nonius FAST'
_diffrn_measurement_method       '\w rotation 0.2\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5944
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.997
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.173
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         2039
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.113
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_obs          0.0380
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+33.8003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0933
_refine_ls_wR_factor_obs         0.0894
_reflns_number_observed          1811
_reflns_number_total             2039
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9700361_3.cif
_cod_data_source_block           W2Cl4(n-PrNH)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^)+(0.0369P)^2^+33.8003P] 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^)+(0.0369P)^2^+33.8003P] 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               4323468