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_4323317
_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         'C16 H42 Cl4 N4 W2'
_chemical_formula_structural     W2Cl4(NEt2)2(NHEt2)2
_chemical_formula_sum            'C16 H42 Cl4 N4 W2'
_chemical_formula_weight         800.04
_chemical_melting_point          ?
_chemical_name_common
;
 cis,cis-Tetrachloro-bis(diethylamido)-bis(diethylamine)
 ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(diethylamido)-(cis,cis)-1,2-
 bis(diethylamine) ditungsten(III) 
;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6704(9)
_cell_length_b                   13.336(1)
_cell_length_c                   17.321(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.6
_cell_measurement_theta_min      17.0
_cell_volume                     2695.8(4)
_computing_cell_refinement       'CAD4 V.5.0'
_computing_data_collection       'CAD4 V.5.0'
_computing_data_reduction        'SDP (Enraf-Nonius, 1979)'
_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      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w
_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  0.0087
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1753
_diffrn_reflns_theta_max         26.93
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'every 300 reflections'
_diffrn_standards_interval_time  'every 3600 sec.'
_diffrn_standards_number         '3 refl. for orient. and 3 refl. for int.'
_exptl_absorpt_coefficient_mu    8.933
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.5887
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(15)
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.098
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1722
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.132
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_obs          0.0224
_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^)+(0.0308P)^2^+3.0493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0560
_refine_ls_wR_factor_obs         0.0539
_reflns_number_observed          1600
_reflns_number_total             1722
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic9610694_2.cif
_cod_data_source_block           W2Cl4(NEt2)2(NHEt2)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^)+(0.0308P)^2^+3.0493P] 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^)+(0.0308P)^2^+3.0493P] 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               4323317