#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:33:56 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179335 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/32/4323273.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_4323273
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Wai-Yeung Wong'
_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         'C13 H34 Cl4 N2 P2 W2'
_chemical_formula_structural     W2Cl4(NHCMe3)2(DMPM)
_chemical_formula_sum            'C13 H34 Cl4 N2 P2 W2'
_chemical_formula_weight         789.86
_chemical_melting_point          ?
_chemical_name_common
;
 cis,cis-Tetrachloro-bis(t-butylamido)-bis(dimethyl-
 phosphino)methane ditungsten(III)
;
_chemical_name_systematic
; 
 1,1,2,2-Tetrachloro-1,2-bis(t-butylamido)-(cis,cis)-1,2-
 bis(dimethylphosphino)methane 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                 109.19(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.807(1)
_cell_length_b                   11.835(2)
_cell_length_c                   15.348(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      10.7
_cell_volume                     2368.6(5)
_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      123(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--2θ
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4346
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.22
_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    10.292
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.4896
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.164
_refine_diff_density_min         -1.992
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_obs          0.0324
_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/[σ²(Fo²)+(0.0407P)²+19.9611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0879
_refine_ls_wR_factor_obs         0.0832
_reflns_number_observed          3763
_reflns_number_total             4163
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic960906z_2.cif
_cod_data_source_block           W2Cl4(NHCMe3)2(DMPM)
_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^)+(0.0407P)^2^+19.9611P] 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^)+(0.0407P)^2^+19.9611P] 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               4323273
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 0.11106(2) 0.93715(2) 0.29468(2) 0.01072(10) Uani 1 d . .
W2 W -0.00980(2) 0.81665(2) 0.32030(2) 0.01201(10) Uani 1 d . .
P1 P -0.03083(14) 1.0596(2) 0.19558(13) 0.0150(4) Uani 1 d . .
P2 P -0.11070(15) 0.8190(2) 0.15191(13) 0.0166(4) Uani 1 d . .
Cl1 Cl 0.25789(13) 0.81603(15) 0.34180(12) 0.0172(4) Uani 1 d . .
Cl2 Cl 0.13613(14) 0.9273(2) 0.14438(12) 0.0190(4) Uani 1 d . .
Cl3 Cl -0.17184(14) 0.9028(2) 0.31388(13) 0.0231(4) Uani 1 d . .
Cl4 Cl 0.02905(14) 0.8364(2) 0.48245(12) 0.0196(4) Uani 1 d . .
N1 N 0.1429(5) 1.0298(5) 0.4012(4) 0.0146(13) Uani 1 d . .
H1 H 0.1047(5) 1.0236(5) 0.4369(4) 0.017 Uiso 1 calc R .
N2 N 0.0549(5) 0.6749(5) 0.3162(4) 0.0168(13) Uani 1 d . .
H2 H 0.1120(5) 0.6776(5) 0.3026(4) 0.020 Uiso 1 calc R .
C1 C -0.0974(6) 1.1497(7) 0.2533(6) 0.023(2) Uani 1 d . .
H1A H -0.1134(6) 1.1063(7) 0.3012(6) 0.035 Uiso 1 calc R .
H1B H -0.1611(6) 1.1775(7) 0.2083(6) 0.035 Uiso 1 calc R .
H1C H -0.0535(6) 1.2139(7) 0.2817(6) 0.035 Uiso 1 calc R .
C2 C -0.0001(6) 1.1602(7) 0.1193(6) 0.023(2) Uani 1 d . .
H2A H 0.0124(6) 1.1197(7) 0.0684(6) 0.034 Uiso 1 calc R .
H2B H 0.0615(6) 1.2027(7) 0.1538(6) 0.034 Uiso 1 calc R .
H2C H -0.0576(6) 1.2126(7) 0.0946(6) 0.034 Uiso 1 calc R .
C3 C -0.1262(6) 0.9675(7) 0.1143(5) 0.022(2) Uani 1 d . .
H3A H -0.1961(6) 0.9934(7) 0.1092(5) 0.026 Uiso 1 calc R .
H3B H -0.1188(6) 0.9734(7) 0.0525(5) 0.026 Uiso 1 calc R .
C4 C -0.0593(6) 0.7433(7) 0.0748(5) 0.022(2) Uani 1 d . .
H4A H 0.0111(6) 0.7685(7) 0.0845(5) 0.034 Uiso 1 calc R .
H4B H -0.1017(6) 0.7581(7) 0.0108(5) 0.034 Uiso 1 calc R .
H4C H -0.0593(6) 0.6620(7) 0.0873(5) 0.034 Uiso 1 calc R .
C5 C -0.2399(6) 0.7629(8) 0.1162(6) 0.030(2) Uani 1 d . .
H5A H -0.2808(6) 0.8050(8) 0.1467(6) 0.045 Uiso 1 calc R .
H5B H -0.2377(6) 0.6829(8) 0.1333(6) 0.045 Uiso 1 calc R .
H5C H -0.2710(6) 0.7704(8) 0.0491(6) 0.045 Uiso 1 calc R .
C6 C 0.2282(5) 1.1118(6) 0.4276(5) 0.0140(15) Uani 1 d . .
C7 C 0.1910(6) 1.2254(6) 0.4495(6) 0.023(2) Uani 1 d . .
H7A H 0.1459(6) 1.2599(6) 0.3926(6) 0.035 Uiso 1 calc R .
H7B H 0.2500(6) 1.2749(6) 0.4773(6) 0.035 Uiso 1 calc R .
H7C H 0.1531(6) 1.2149(6) 0.4929(6) 0.035 Uiso 1 calc R .
C8 C 0.2712(6) 1.1249(7) 0.3478(5) 0.024(2) Uani 1 d . .
H8A H 0.3292(6) 1.1775(7) 0.3659(5) 0.036 Uiso 1 calc R .
H8B H 0.2176(6) 1.1542(7) 0.2934(5) 0.036 Uiso 1 calc R .
H8C H 0.2944(6) 1.0511(7) 0.3333(5) 0.036 Uiso 1 calc R .
C9 C 0.3120(6) 1.0652(7) 0.5121(5) 0.022(2) Uani 1 d . .
H9A H 0.3680(6) 1.1201(7) 0.5329(5) 0.033 Uiso 1 calc R .
H9B H 0.3383(6) 0.9942(7) 0.4957(5) 0.033 Uiso 1 calc R .
H9C H 0.2835(6) 1.0514(7) 0.5617(5) 0.033 Uiso 1 calc R .
C10 C 0.0206(6) 0.5622(6) 0.3332(5) 0.019(2) Uani 1 d . .
C11 C 0.0945(7) 0.5219(7) 0.4264(6) 0.026(2) Uani 1 d . .
H11A H 0.0746(7) 0.4460(7) 0.4397(6) 0.038 Uiso 1 calc R .
H11B H 0.0916(7) 0.5741(7) 0.4751(6) 0.038 Uiso 1 calc R .
H11C H 0.1645(7) 0.5199(7) 0.4239(6) 0.038 Uiso 1 calc R .
C12 C -0.0880(7) 0.5688(8) 0.3364(7) 0.034(2) Uani 1 d . .
H12A H -0.1090(7) 0.4943(8) 0.3515(7) 0.050 Uiso 1 calc R .
H12B H -0.1346(7) 0.5931(8) 0.2762(7) 0.050 Uiso 1 calc R .
H12C H -0.0905(7) 0.6234(8) 0.3837(7) 0.050 Uiso 1 calc R .
C13 C 0.0269(8) 0.4816(7) 0.2588(6) 0.033(2) Uani 1 d . .
H13A H 0.0021(8) 0.4069(7) 0.2694(6) 0.049 Uiso 1 calc R .
H13B H 0.0983(8) 0.4755(7) 0.2605(6) 0.049 Uiso 1 calc R .
H13C H -0.0155(8) 0.5100(7) 0.1984(6) 0.049 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'
Cl Cl 0.1484 0.1585 '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'
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'
H H 0.0000 0.0000 '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 100.7(2) . . y
N1 W1 Cl1 98.8(2) . . y
W2 W1 Cl1 99.52(5) . . y
N1 W1 Cl2 140.9(2) . . y
W2 W1 Cl2 117.55(5) . . y
Cl1 W1 Cl2 83.56(6) . . y
N1 W1 P1 95.9(2) . . y
W2 W1 P1 89.77(5) . . y
Cl1 W1 P1 160.85(6) . . y
Cl2 W1 P1 77.29(6) . . y
N2 W2 W1 99.4(2) . . y
N2 W2 Cl4 100.0(2) . . y
W1 W2 Cl4 100.91(5) . . y
N2 W2 Cl3 143.2(2) . . y
W1 W2 Cl3 115.98(5) . . y
Cl4 W2 Cl3 83.64(7) . . y
N2 W2 P2 94.8(2) . . y
W1 W2 P2 90.30(5) . . y
Cl4 W2 P2 159.65(7) . . y
Cl3 W2 P2 76.16(7) . . y
C2 P1 C1 101.1(4) . . n
C2 P1 C3 102.6(4) . . n
C1 P1 C3 108.3(4) . . n
C2 P1 W1 117.9(3) . . n
C1 P1 W1 117.6(3) . . n
C3 P1 W1 108.1(3) . . n
C4 P2 C5 100.3(4) . . n
C4 P2 C3 107.4(4) . . n
C5 P2 C3 104.7(4) . . n
C4 P2 W2 117.8(3) . . n
C5 P2 W2 117.9(3) . . n
C3 P2 W2 107.6(3) . . n
C6 N1 W1 123.7(5) . . n
C10 N2 W2 127.7(5) . . n
P2 C3 P1 111.6(4) . . n
N1 C6 C7 110.3(6) . . n
N1 C6 C9 108.0(6) . . n
C7 C6 C9 110.4(6) . . n
N1 C6 C8 109.3(6) . . n
C7 C6 C8 109.6(6) . . n
C9 C6 C8 109.2(6) . . n
N2 C10 C13 109.8(6) . . n
N2 C10 C12 109.7(7) . . n
C13 C10 C12 111.1(7) . . n
N2 C10 C11 107.1(6) . . n
C13 C10 C11 108.8(7) . . n
C12 C10 C11 110.3(7) . . n
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 1.896(6) . y
W1 W2 2.3247(4) . y
W1 Cl1 2.392(2) . y
W1 Cl2 2.445(2) . y
W1 P1 2.508(2) . y
W2 N2 1.911(6) . y
W2 Cl4 2.379(2) . y
W2 Cl3 2.431(2) . y
W2 P2 2.501(2) . y
P1 C2 1.815(8) . n
P1 C1 1.818(8) . n
P1 C3 1.844(8) . n
P2 C4 1.806(8) . n
P2 C5 1.811(8) . n
P2 C3 1.840(8) . n
N1 C6 1.476(9) . n
N2 C10 1.467(9) . n
C6 C7 1.516(10) . n
C6 C9 1.529(10) . n
C6 C8 1.535(10) . n
C10 C13 1.512(11) . n
C10 C12 1.519(12) . n
C10 C11 1.535(10) . n
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
N1 W1 W2 Cl3 67.4(2) . . . . y
P1 W1 W2 Cl3 -28.50(7) . . . . y
Cl1 W1 W2 Cl3 168.32(7) . . . . y
Cl2 W1 W2 Cl3 -104.01(7) . . . . y
N1 W1 W2 Cl4 -20.8(2) . . . . y
P1 W1 W2 Cl4 -116.69(7) . . . . y
Cl1 W1 W2 Cl4 80.13(7) . . . . y
Cl2 W1 W2 Cl4 167.80(7) . . . . y
N1 W1 W2 N2 -122.9(3) . . . . y
P1 W1 W2 N2 141.1(2) . . . . y
Cl1 W1 W2 N2 -22.0(2) . . . . y
Cl2 W1 W2 N2 65.6(2) . . . . y
N1 W1 W2 P2 142.2(2) . . . . y
P1 W1 W2 P2 46.22(7) . . . . y
Cl1 W1 W2 P2 -116.95(7) . . . . y
Cl2 W1 W2 P2 -29.29(7) . . . . y
