#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:34:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179336 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/33/4323337.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323337
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Wai-Yeung Wong'
_publ_section_title
;
 W2Cl4(NR2)2(PR'3)2 Molecules. 5. Preparation and Characterization of
 W2Cl4(NEt2)2(L-L) (L-L = dmpm, dmpe, dppe), W2Cl4(NBu2)2(L-L) (L-L =
 dmpm, dmpe), and W2Cl4(NHex2)2(dmpm). First Complexes with Bridging
 Diphosphine Ligands in a cis,trans-Stereochemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              902
_journal_page_last               912
_journal_paper_doi               10.1021/ic961151z
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C22 H52 Cl4 N2 P2 W2'
_chemical_formula_structural     cis,trans-W2Cl4(n-Bu2N)2(DMPE)
_chemical_formula_sum            'C22 H52 Cl4 N2 P2 W2'
_chemical_formula_weight         916.10
_chemical_name_common
;
 cis,trans-Tetrachloro-bis(dibutylamido)-bis(dimethylphosphino)ethane
 ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(dibutylamido)-(cis,trans)-1,2-
 bis(dimethylphosphino)ethane 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                 97.220(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.465(1)
_cell_length_b                   34.545(7)
_cell_length_c                   10.177(4)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     3301.2(15)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'MADNES (Enraf-Nonius, 1989)'
_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       'ω rotation 0.2°'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0929
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2546
_diffrn_reflns_theta_max         21.72
_diffrn_reflns_theta_min         2.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.398
_exptl_absorpt_correction_T_max  0.7969
_exptl_absorpt_correction_T_min  0.6097
_exptl_absorpt_correction_type
;
 empirical (R.H.Blessing Acta Cryst., 1995, A51, 33-38)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.160
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         2545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_restrained_S_obs      1.160
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_obs          0.0470
_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/[σ²(Fo²)+(0.0456P)²+0.5068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1298
_refine_ls_wR_factor_obs         0.1063
_reflns_number_observed          1934
_reflns_number_total             2546
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961151z_9.cif
_cod_data_source_block           W2Cl4(NBu2)2(DMPE)
_cod_depositor_comments
;
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^)+(0.0456P)^2^+0.5068P] 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^)+(0.0456P)^2^+0.5068P] 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        3301(2)
_cod_database_code               4323337
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W1 W 0.51744(5) 0.169758(14) 0.05295(5) 0.0187(3) Uani 1 d . .
W2 W 0.36741(5) 0.135403(15) 0.17371(5) 0.0224(3) Uani 1 d . .
P1 P 0.6794(3) 0.19768(10) 0.2457(3) 0.0222(8) Uani 1 d . .
P2 P 0.3370(4) 0.18790(11) 0.3505(3) 0.0270(9) Uani 1 d . .
Cl1 Cl 0.4002(4) 0.16856(9) -0.1693(3) 0.0366(10) Uani 1 d . .
Cl2 Cl 0.4547(3) 0.23831(9) 0.0437(3) 0.0308(8) Uani 1 d . .
Cl3 Cl 0.5007(4) 0.10826(10) 0.3648(3) 0.0355(9) Uani 1 d . .
Cl4 Cl 0.1407(3) 0.16025(11) 0.0925(4) 0.0396(9) Uani 1 d . .
N1 N 0.6623(10) 0.1330(3) 0.0278(10) 0.021(3) Uani 1 d . .
N2 N 0.3332(11) 0.0866(3) 0.0792(10) 0.031(3) Uani 1 d . .
C1 C 0.8016(13) 0.2316(4) 0.1876(12) 0.031(3) Uani 1 d . .
H1A H 0.7488(13) 0.2512(4) 0.1340(12) 0.040(11) Uiso 1 calc R .
H1B H 0.8644(13) 0.2181(4) 0.1348(12) 0.040(11) Uiso 1 calc R .
H1C H 0.8577(13) 0.2437(4) 0.2628(12) 0.040(11) Uiso 1 calc R .
C2 C 0.8028(14) 0.1654(4) 0.3399(12) 0.033(4) Uani 1 d . .
H2A H 0.7505(14) 0.1450(4) 0.3782(12) 0.040(11) Uiso 1 calc R .
H2B H 0.8588(14) 0.1797(4) 0.4100(12) 0.040(11) Uiso 1 calc R .
H2C H 0.8656(14) 0.1540(4) 0.2820(12) 0.040(11) Uiso 1 calc R .
C3 C 0.6016(13) 0.2262(4) 0.3687(12) 0.032(4) Uani 1 d . .
H3A H 0.6792(13) 0.2369(4) 0.4310(12) 0.035(18) Uiso 1 calc R .
H3B H 0.5505(13) 0.2481(4) 0.3235(12) 0.035(18) Uiso 1 calc R .
C4 C 0.4979(13) 0.2044(4) 0.4492(13) 0.038(4) Uani 1 d . .
H4A H 0.4718(13) 0.2216(4) 0.5188(13) 0.035(18) Uiso 1 calc R .
H4B H 0.5474(13) 0.1820(4) 0.4925(13) 0.035(18) Uiso 1 calc R .
C5 C 0.2417(14) 0.2332(4) 0.3044(13) 0.035(4) Uani 1 d . .
H5A H 0.2897(14) 0.2470(4) 0.2397(13) 0.040(11) Uiso 1 calc R .
H5B H 0.2403(14) 0.2493(4) 0.3826(13) 0.040(11) Uiso 1 calc R .
H5C H 0.1447(14) 0.2274(4) 0.2667(13) 0.040(11) Uiso 1 calc R .
C6 C 0.2358(16) 0.1663(4) 0.4692(14) 0.046(4) Uani 1 d . .
H6A H 0.1465(16) 0.1565(4) 0.4242(14) 0.040(11) Uiso 1 calc R .
H6B H 0.2166(16) 0.1856(4) 0.5340(14) 0.040(11) Uiso 1 calc R .
H6C H 0.2897(16) 0.1451(4) 0.5136(14) 0.040(11) Uiso 1 calc R .
C7 C 0.7595(14) 0.1493(4) -0.0604(12) 0.028(3) Uani 1 d . .
H7A H 0.8573(14) 0.1484(4) -0.0155(12) 0.047(8) Uiso 1 calc R .
H7B H 0.7348(14) 0.1765(4) -0.0785(12) 0.047(8) Uiso 1 calc R .
C8 C 0.7520(16) 0.1274(4) -0.1914(13) 0.038(4) Uani 1 d . .
H8A H 0.6535(16) 0.1195(4) -0.2203(13) 0.047(8) Uiso 1 calc R .
H8B H 0.8108(16) 0.1040(4) -0.1794(13) 0.047(8) Uiso 1 calc R .
C9 C 0.8056(18) 0.1534(5) -0.2973(15) 0.056(5) Uani 1 d . .
H9A H 0.7979(18) 0.1391(5) -0.3810(15) 0.047(8) Uiso 1 calc R .
H9B H 0.7430(18) 0.1760(5) -0.3109(15) 0.047(8) Uiso 1 calc R .
C10 C 0.9551(17) 0.1671(4) -0.2644(15) 0.053(5) Uani 1 d . .
H10A H 0.9806(17) 0.1832(4) -0.3357(15) 0.073(15) Uiso 1 calc R .
H10B H 1.0185(17) 0.1449(4) -0.2532(15) 0.073(15) Uiso 1 calc R .
H10C H 0.9635(17) 0.1819(4) -0.1829(15) 0.073(15) Uiso 1 calc R .
C11 C 0.6945(13) 0.0921(4) 0.0697(13) 0.033(3) Uani 1 d . .
H11A H 0.6585(13) 0.0752(4) -0.0042(13) 0.047(8) Uiso 1 calc R .
H11B H 0.6401(13) 0.0862(4) 0.1430(13) 0.047(8) Uiso 1 calc R .
C12 C 0.8491(14) 0.0814(4) 0.1131(16) 0.047(4) Uani 1 d . .
H12A H 0.8933(14) 0.1007(4) 0.1758(16) 0.047(8) Uiso 1 calc R .
H12B H 0.9018(14) 0.0809(4) 0.0361(16) 0.047(8) Uiso 1 calc R .
C13 C 0.8546(16) 0.0417(5) 0.1783(17) 0.057(5) Uani 1 d . .
H13A H 0.7868(16) 0.0245(5) 0.1260(17) 0.047(8) Uiso 1 calc R .
H13B H 0.9501(16) 0.0308(5) 0.1774(17) 0.047(8) Uiso 1 calc R .
C14 C 0.8213(21) 0.0424(5) 0.3158(18) 0.082(6) Uani 1 d . .
H14A H 0.8266(21) 0.0164(5) 0.3516(18) 0.073(15) Uiso 1 calc R .
H14B H 0.7260(21) 0.0526(5) 0.3175(18) 0.073(15) Uiso 1 calc R .
H14C H 0.8894(21) 0.0588(5) 0.3689(18) 0.073(15) Uiso 1 calc R .
C15 C 0.3565(14) 0.0736(4) -0.0521(12) 0.034(4) Uani 1 d . .
H15A H 0.3913(14) 0.0469(4) -0.0466(12) 0.047(8) Uiso 1 calc R .
H15B H 0.4304(14) 0.0897(4) -0.0839(12) 0.047(8) Uiso 1 calc R .
C16 C 0.2212(15) 0.0756(4) -0.1522(13) 0.043(4) Uani 1 d . .
H16A H 0.1512(15) 0.0570(4) -0.1271(13) 0.047(8) Uiso 1 calc R .
H16B H 0.1796(15) 0.1016(4) -0.1506(13) 0.047(8) Uiso 1 calc R .
C17 C 0.2545(16) 0.0666(5) -0.2918(14) 0.056(5) Uani 1 d . .
H17A H 0.3236(16) 0.0855(5) -0.3167(14) 0.047(8) Uiso 1 calc R .
H17B H 0.2983(16) 0.0409(5) -0.2922(14) 0.047(8) Uiso 1 calc R .
C18 C 0.1230(21) 0.0675(5) -0.3939(17) 0.083(6) Uani 1 d . .
H18A H 0.1498(21) 0.0616(5) -0.4806(17) 0.073(15) Uiso 1 calc R .
H18B H 0.0803(21) 0.0930(5) -0.3954(17) 0.073(15) Uiso 1 calc R .
H18C H 0.0550(21) 0.0484(5) -0.3710(17) 0.073(15) Uiso 1 calc R .
C19 C 0.2549(14) 0.0578(4) 0.1503(14) 0.040(4) Uani 1 d . .
H19A H 0.1741(14) 0.0480(4) 0.0898(14) 0.047(8) Uiso 1 calc R .
H19B H 0.2169(14) 0.0706(4) 0.2242(14) 0.047(8) Uiso 1 calc R .
C20 C 0.3479(16) 0.0235(4) 0.2042(14) 0.044(4) Uani 1 d . .
H20A H 0.4332(16) 0.0332(4) 0.2589(14) 0.047(8) Uiso 1 calc R .
H20B H 0.3784(16) 0.0089(4) 0.1302(14) 0.047(8) Uiso 1 calc R .
C21 C 0.2625(21) -0.0038(5) 0.2895(18) 0.072(5) Uani 1 d . .
H21A H 0.2229(21) 0.0114(5) 0.3574(18) 0.047(8) Uiso 1 calc R .
H21B H 0.1833(21) -0.0158(5) 0.2326(18) 0.047(8) Uiso 1 calc R .
C22 C 0.3571(21) -0.0342(5) 0.3534(17) 0.076(6) Uani 1 d . .
H22A H 0.3033(21) -0.0509(5) 0.4057(17) 0.073(15) Uiso 1 calc R .
H22B H 0.4347(21) -0.0223(5) 0.4106(17) 0.073(15) Uiso 1 calc R .
H22C H 0.3952(21) -0.0495(5) 0.2860(17) 0.073(15) Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 W1 W2 103.2(3) . . yes
N1 W1 Cl1 96.7(3) . . yes
W2 W1 Cl1 104.48(9) . . yes
N1 W1 Cl2 144.6(3) . . yes
W2 W1 Cl2 110.77(8) . . yes
Cl1 W1 Cl2 84.19(11) . . yes
N1 W1 P1 89.0(3) . . yes
W2 W1 P1 97.83(8) . . yes
Cl1 W1 P1 154.96(11) . . yes
Cl2 W1 P1 77.31(11) . . yes
N2 W2 W1 104.8(3) . . yes
N2 W2 Cl4 93.1(3) . . yes
W1 W2 Cl4 102.62(9) . . yes
N2 W2 Cl3 95.8(3) . . yes
W1 W2 Cl3 109.79(8) . . yes
Cl4 W2 Cl3 142.77(12) . . yes
N2 W2 P2 157.1(3) . . yes
W1 W2 P2 97.97(8) . . yes
Cl4 W2 P2 79.26(12) . . yes
Cl3 W2 P2 78.58(12) . . yes
C1 P1 C2 100.2(6) . . no
C1 P1 C3 101.9(6) . . no
C2 P1 C3 105.1(6) . . no
C1 P1 W1 110.3(4) . . no
C2 P1 W1 117.8(5) . . no
C3 P1 W1 118.9(4) . . no
C6 P2 C4 103.9(7) . . no
C6 P2 C5 103.9(6) . . no
C4 P2 C5 103.0(7) . . no
C6 P2 W2 106.9(5) . . no
C4 P2 W2 116.5(4) . . no
C5 P2 W2 120.8(5) . . no
C7 N1 C11 114.5(9) . . no
C7 N1 W1 109.9(7) . . no
C11 N1 W1 135.5(8) . . no
C15 N2 C19 112.7(10) . . no
C15 N2 W2 133.3(9) . . no
C19 N2 W2 113.7(8) . . no
C4 C2 P1 116.0(9) . . no
C3 C5 P2 113.9(9) . . no
N1 C7 C8 112.1(11) . . no
C7 C8 C9 109.7(11) . . no
C10 C9 C8 114.5(13) . . no
N1 C11 C12 117.9(11) . . no
C11 C12 C13 109.0(12) . . no
C14 C13 C12 113.5(14) . . no
N2 C15 C16 112.7(11) . . no
C17 C16 C15 110.9(12) . . no
C18 C17 C16 112.7(14) . . no
N2 C19 C20 113.1(11) . . no
C19 C20 C21 110.4(12) . . no
C22 C21 C20 110.2(15) . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 N1 1.910(9) . yes
W1 W2 2.3182(8) . yes
W1 Cl1 2.391(3) . yes
W1 Cl2 2.440(3) . yes
W1 P1 2.525(3) . yes
W2 N2 1.948(10) . yes
W2 Cl4 2.362(3) . yes
W2 Cl3 2.374(3) . yes
W2 P2 2.596(4) . yes
P1 C1 1.797(12) . no
P1 C2 1.801(13) . no
P1 C3 1.820(12) . no
P2 C6 1.795(14) . no
P2 C4 1.808(13) . no
P2 C5 1.839(12) . no
N1 C7 1.48(2) . no
N1 C11 1.49(2) . no
N2 C15 1.45(2) . no
N2 C19 1.48(2) . no
C3 C4 1.55(2) . no
C7 C8 1.53(2) . no
C8 C9 1.54(2) . no
C9 C10 1.49(2) . no
C11 C12 1.52(2) . no
C12 C13 1.52(2) . no
C13 C14 1.47(2) . no
C15 C16 1.53(2) . no
C16 C17 1.53(2) . no
C17 C18 1.52(2) . no
C19 C20 1.53(2) . no
C20 C21 1.57(2) . no
C21 C22 1.48(2) . no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 W1 W2 P2 43.22(11) . . . . yes
P1 W1 W2 N2 -139.3(3) . . . . no
P1 W1 W2 Cl3 -37.44(12) . . . . yes
P1 W1 W2 Cl4 123.93(12) . . . . no
N1 W1 W2 P2 134.0(3) . . . . no
N1 W1 W2 N2 -48.5(4) . . . . yes
N1 W1 W2 Cl3 53.4(3) . . . . yes
N1 W1 W2 Cl4 -145.3(3) . . . . no
Cl2 W1 W2 P2 -36.11(11) . . . . yes
Cl2 W1 W2 N2 141.3(3) . . . . no
Cl2 W1 W2 Cl3 -116.78(12) . . . . no
Cl2 W1 W2 Cl4 44.60(12) . . . . yes
Cl1 W1 W2 P2 -125.31(12) . . . . no
Cl1 W1 W2 N2 52.1(3) . . . . yes
Cl1 W1 W2 Cl3 154.02(13) . . . . no
Cl1 W1 W2 Cl4 -44.61(12) . . . . yes
