#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:33:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179334 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/31/4323156.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_4323156
loop_
_publ_author_name
'Jesper Bendix'
'Anders Bøgevig'
_publ_section_title
;
 Synthesis and Characterization of a Stable trans-Dioxo Tungsten(IV)
 Complex and Series of Mono-Oxo Molybdenum(IV) and Tungsten(IV) Complexes.
 Structural and Electronic Effects of π-Bonding in
 trans-[M(O)(X)(dppe)2]+/0 Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5992
_journal_page_last               6001
_journal_paper_doi               10.1021/ic980342u
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C54 H56 O4 P4 W'
_chemical_formula_weight         1076.72
_chemical_name_systematic
; 
trans-dioxo-bis(diphenylphosphinoethane)tungsten(IV) dimethanol solvate.
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
98-03-15   edited for submission to Inorg. Chem. These data pertains to the 
compound labeled 11 in the manuscript.
;
_cell_angle_alpha                110.864(19)
_cell_angle_beta                 99.05(2)
_cell_angle_gamma                110.244(19)
_cell_formula_units_Z            1
_cell_length_a                   9.464(2)
_cell_length_b                   11.429(2)
_cell_length_c                   13.126(3)
_cell_measurement_temperature    122(2)
_cell_volume                     1179.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6857
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    2.631
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             546
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0195P)²+0.2698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                6845
_reflns_number_total             6857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980342u_1.cif
_cod_data_source_block           fh454_abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.2698P] 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^)+(0.0195P)^2^+0.2698P] 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        1179.4(5)
_cod_database_code               4323156
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.0000 0.0000 0.0000 0.00891(3) Uani 1 d S . .
P1 P 0.24162(4) 0.19188(4) 0.16366(3) 0.01085(7) Uani 1 d . . .
P2 P 0.19430(4) 0.04739(4) -0.10527(3) 0.01126(7) Uani 1 d . . .
O1 O 0.08648(13) -0.11295(11) 0.02237(9) 0.0135(2) Uani 1 d . . .
C1 C 0.41736(18) 0.22327(17) 0.11213(14) 0.0151(3) Uani 1 d . . .
H1A H 0.429(3) 0.303(2) 0.100(2) 0.023(6) Uiso 1 d . . .
H1B H 0.513(3) 0.245(3) 0.178(2) 0.027(6) Uiso 1 d . . .
C11A C 0.26229(18) 0.36857(15) 0.23628(13) 0.0135(3) Uani 1 d . . .
C16A C 0.1862(2) 0.41743(17) 0.17269(14) 0.0172(3) Uani 1 d . . .
H16A H 0.120(3) 0.353(2) 0.095(2) 0.019(5) Uiso 1 d . . .
C15A C 0.2104(2) 0.55589(18) 0.22215(16) 0.0203(3) Uani 1 d . . .
H15A H 0.165(3) 0.588(3) 0.178(2) 0.029(6) Uiso 1 d . . .
C14A C 0.3074(2) 0.64456(18) 0.33482(16) 0.0211(3) Uani 1 d . . .
H14A H 0.326(3) 0.735(3) 0.365(2) 0.027(6) Uiso 1 d . . .
C13A C 0.3821(2) 0.59668(18) 0.39908(15) 0.0220(3) Uani 1 d . . .
H13A H 0.445(3) 0.654(3) 0.472(2) 0.025(6) Uiso 1 d . . .
C12A C 0.3607(2) 0.45915(17) 0.34967(14) 0.0188(3) Uani 1 d . . .
H12A H 0.413(3) 0.430(2) 0.394(2) 0.026(6) Uiso 1 d . . .
C11B C 0.28688(18) 0.14385(16) 0.27858(13) 0.0149(3) Uani 1 d . . .
C16B C 0.2119(2) 0.16447(18) 0.36266(15) 0.0197(3) Uani 1 d . . .
H16B H 0.148(3) 0.211(3) 0.363(2) 0.030(6) Uiso 1 d . . .
C15B C 0.2306(2) 0.1137(2) 0.44342(16) 0.0266(4) Uani 1 d . . .
H15B H 0.177(3) 0.131(3) 0.498(2) 0.030(6) Uiso 1 d . . .
C14B C 0.3222(2) 0.0410(2) 0.43939(18) 0.0300(4) Uani 1 d . . .
H14B H 0.338(3) 0.004(3) 0.492(3) 0.046(8) Uiso 1 d . . .
C13B C 0.3948(2) 0.0187(2) 0.35569(18) 0.0280(4) Uani 1 d . . .
H13B H 0.453(4) -0.037(3) 0.349(3) 0.045(8) Uiso 1 d . . .
C12B C 0.3784(2) 0.07046(18) 0.27537(15) 0.0208(3) Uani 1 d . . .
H12B H 0.429(3) 0.055(2) 0.222(2) 0.025(6) Uiso 1 d . . .
C2 C 0.38753(18) 0.10222(17) -0.00167(13) 0.0143(3) Uani 1 d . . .
H2A H 0.374(3) 0.020(2) 0.0065(19) 0.019(5) Uiso 1 d . . .
H2B H 0.475(2) 0.129(2) -0.0326(18) 0.013(5) Uiso 1 d . . .
C21A C 0.22106(18) 0.18258(16) -0.15260(13) 0.0138(3) Uani 1 d . . .
C22A C 0.0880(2) 0.20079(18) -0.19235(15) 0.0180(3) Uani 1 d . . .
H22A H -0.012(3) 0.149(2) -0.1885(19) 0.019(5) Uiso 1 d . . .
C23A C 0.1011(2) 0.2933(2) -0.24024(17) 0.0238(3) Uani 1 d . . .
H23A H 0.010(3) 0.305(3) -0.269(2) 0.033(7) Uiso 1 d . . .
C24A C 0.2465(3) 0.3692(2) -0.24707(18) 0.0263(4) Uani 1 d . . .
H24A H 0.254(3) 0.432(3) -0.281(2) 0.037(7) Uiso 1 d . . .
C25A C 0.3797(2) 0.3538(2) -0.20611(18) 0.0253(4) Uani 1 d . . .
H25A H 0.480(3) 0.406(3) -0.210(2) 0.031(6) Uiso 1 d . . .
C26A C 0.3671(2) 0.25976(18) -0.15970(16) 0.0202(3) Uani 1 d . . .
H26A H 0.463(3) 0.250(3) -0.134(2) 0.027(6) Uiso 1 d . . .
C21B C 0.18402(18) -0.09720(16) -0.23034(14) 0.0150(3) Uani 1 d . . .
C22B C 0.1609(2) -0.22019(19) -0.22197(15) 0.0221(3) Uani 1 d . . .
H22B H 0.154(3) -0.224(3) -0.154(2) 0.034(7) Uiso 1 d . . .
C23B C 0.1444(3) -0.3362(2) -0.31599(18) 0.0277(4) Uani 1 d . . .
H23B H 0.123(3) -0.422(3) -0.312(2) 0.043(8) Uiso 1 d . . .
C24B C 0.1496(2) -0.3309(2) -0.41903(17) 0.0292(4) Uani 1 d . . .
H24B H 0.141(3) -0.409(3) -0.481(2) 0.028(6) Uiso 1 d . . .
C25B C 0.1682(3) -0.2102(2) -0.42913(17) 0.0316(4) Uani 1 d . . .
H25B H 0.172(3) -0.207(3) -0.498(2) 0.037(7) Uiso 1 d . . .
C26B C 0.1868(2) -0.09273(19) -0.33475(16) 0.0245(4) Uani 1 d . . .
H26B H 0.200(3) -0.011(3) -0.343(2) 0.031(6) Uiso 1 d . . .
O O 0.26678(17) -0.23728(15) 0.07213(13) 0.0282(3) Uani 1 d . . .
H H 0.202(3) -0.209(3) 0.054(2) 0.036(7) Uiso 1 d . . .
C C 0.2146(3) -0.3695(2) -0.01794(19) 0.0287(4) Uani 1 d . . .
H1 H 0.270(3) -0.425(3) 0.002(2) 0.039(7) Uiso 1 d . . .
H2 H 0.101(5) -0.429(4) -0.041(3) 0.075(11) Uiso 1 d . . .
H3 H 0.235(5) -0.366(4) -0.093(4) 0.094(14) Uiso 1 d . . .
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'
O O 0.0106 0.0060 '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'
W W -0.8490 6.8722 '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
O1 W O1 180.0 2 . y
O1 W P2 84.10(4) 2 2 y
O1 W P2 95.90(4) . 2 y
O1 W P2 95.90(4) 2 . ?
O1 W P2 84.10(4) . . ?
P2 W P2 180.0 2 . ?
O1 W P1 95.60(4) 2 . y
O1 W P1 84.40(4) . . y
P2 W P1 100.51(3) 2 . y
P2 W P1 79.49(3) . . y
O1 W P1 84.40(4) 2 2 ?
O1 W P1 95.60(4) . 2 ?
P2 W P1 79.49(3) 2 2 ?
P2 W P1 100.51(3) . 2 ?
P1 W P1 180.0 . 2 ?
C11B P1 C11A 104.99(8) . . ?
C11B P1 C1 105.69(8) . . ?
C11A P1 C1 100.96(7) . . ?
C11B P1 W 111.62(5) . . ?
C11A P1 W 122.87(6) . . ?
C1 P1 W 109.09(6) . . ?
C21A P2 C21B 103.37(7) . . ?
C21A P2 C2 106.13(8) . . ?
C21B P2 C2 102.32(8) . . ?
C21A P2 W 119.69(5) . . ?
C21B P2 W 119.14(6) . . ?
C2 P2 W 104.23(5) . . ?
C2 C1 P1 112.54(11) . . ?
C16A C11A C12A 119.28(15) . . ?
C16A C11A P1 118.16(12) . . ?
C12A C11A P1 122.37(12) . . ?
C11A C16A C15A 119.91(16) . . ?
C14A C15A C16A 120.32(16) . . ?
C15A C14A C13A 120.21(16) . . ?
C14A C13A C12A 119.82(16) . . ?
C13A C12A C11A 120.45(16) . . ?
C12B C11B C16B 119.40(15) . . ?
C12B C11B P1 120.74(13) . . ?
C16B C11B P1 119.32(12) . . ?
C15B C16B C11B 120.13(17) . . ?
C14B C15B C16B 119.89(19) . . ?
C13B C14B C15B 120.24(17) . . ?
C14B C13B C12B 120.31(18) . . ?
C13B C12B C11B 120.02(18) . . ?
C1 C2 P2 110.37(11) . . ?
C22A C21A C26A 119.36(15) . . ?
C22A C21A P2 118.54(12) . . ?
C26A C21A P2 121.86(12) . . ?
C23A C22A C21A 120.02(16) . . ?
C24A C23A C22A 120.18(17) . . ?
C25A C24A C23A 120.26(16) . . ?
C24A C25A C26A 119.93(17) . . ?
C25A C26A C21A 120.22(16) . . ?
C22B C21B C26B 119.20(15) . . ?
C22B C21B P2 117.59(13) . . ?
C26B C21B P2 123.04(13) . . ?
C23B C22B C21B 120.39(17) . . ?
C24B C23B C22B 120.30(18) . . ?
C23B C24B C25B 119.73(17) . . ?
C24B C25B C26B 120.32(18) . . ?
C21B C26B C25B 120.03(18) . . ?
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
W O1 1.8298(11) 2 y
W O1 1.8298(11) . y
W P2 2.4955(7) 2 y
W P2 2.4955(7) . y
W P1 2.5065(12) . y
W P1 2.5065(12) 2 y
P1 C11B 1.8193(16) . ?
P1 C11A 1.8226(16) . ?
P1 C1 1.8617(16) . ?
P2 C21A 1.8165(16) . ?
P2 C21B 1.8280(17) . ?
P2 C2 1.8450(17) . ?
C1 C2 1.533(2) . ?
C11A C16A 1.396(2) . ?
C11A C12A 1.398(2) . ?
C16A C15A 1.396(2) . ?
C15A C14A 1.385(3) . ?
C14A C13A 1.385(3) . ?
C13A C12A 1.394(2) . ?
C11B C12B 1.394(2) . ?
C11B C16B 1.398(2) . ?
C16B C15B 1.394(2) . ?
C15B C14B 1.388(3) . ?
C14B C13B 1.379(3) . ?
C13B C12B 1.393(2) . ?
C21A C22A 1.397(2) . ?
C21A C26A 1.397(2) . ?
C22A C23A 1.391(2) . ?
C23A C24A 1.387(3) . ?
C24A C25A 1.384(3) . ?
C25A C26A 1.393(2) . ?
C21B C22B 1.393(2) . ?
C21B C26B 1.394(2) . ?
C22B C23B 1.391(3) . ?
C23B C24B 1.383(3) . ?
C24B C25B 1.386(3) . ?
C25B C26B 1.397(3) . ?
O C 1.398(3) . ?
