#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/65/2006509.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006509
loop_
_publ_author_name
'Dahlenburg, Lutz'
'Herbst, Konrad'
'Knoch, Falk'
_publ_section_title
;
 Tetracarbonylbis[(2-methoxyphenyl)diphenylphosphine-P]tungsten
 Dichloromethane 0.25-Solvate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1188
_journal_page_last               1190
_journal_paper_doi               10.1107/S0108270197006136
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[W(C19 H17 O P)2 (C O)4].0.25C H2 Cl2'
_chemical_formula_sum            'C42.25 H34.5 Cl0.5 O6 P2 W'
_chemical_formula_weight         901.71
_chemical_name_systematic
;
 Tetracarbonylbis[(2-methoxyphenyl)diphenylphosphane]tungsten-dichloromethane
 (4/1)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           'SHELXL93 (Sheldrick, 1993)'
_cell_angle_alpha                90.00
_cell_angle_beta                 109.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.524(8)
_cell_length_b                   15.174(5)
_cell_length_c                   10.978(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      14
_cell_volume                     4018(2)
_computing_cell_refinement       P3/V
_computing_data_collection       'P3/V (Siemens, 1989)'
_computing_data_reduction        SHELXTL-Plus
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5641
_diffrn_reflns_theta_max         27.28
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.032
_exptl_absorpt_correction_T_max  0.22
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type
;
\y scans (SHELXTL-Plus; Sheldrick, 1990)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1794
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.838
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.165
_refine_ls_goodness_of_fit_obs   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.164
_refine_ls_restrained_S_obs      1.231
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_obs          .0402
_refine_ls_shift/esd_max         0.035
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0927P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1478
_refine_ls_wR_factor_obs         .1453
_reflns_number_observed          3878
_reflns_number_total             4461
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1228.cif
_cod_data_source_block           herb04
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4019(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C42.25 H34.50 Cl0.50 O6 P2 W'
_cod_database_code               2006509
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
W .0000 .26066(2) .2500 .03459(15) Uani d S 1 . W
P -.10270(7) .25432(9) .1520(2) .0354(3) Uani d . 1 . P
O1 .0230(3) .4161(4) .0840(7) .085(2) Uani d . 1 . O
O2 .0084(3) .1150(4) .0475(6) .077(2) Uani d . 1 . O
O3 -.0907(2) .0625(3) .1493(5) .0523(12) Uani d . 1 . O
C1 .0131(3) .3578(5) .1395(8) .052(2) Uani d . 1 . C
C2 .0056(3) .1671(5) .1215(8) .051(2) Uani d . 1 . C
C3 -.1312(2) .1807(4) .0145(6) .0400(13) Uani d . 1 . C
C4 -.1199(3) .0892(5) .0266(7) .0450(15) Uani d . 1 . C
C5 -.1391(3) .0323(5) -.0786(8) .056(2) Uani d . 1 . C
H5 -.1308(3) -.0275(5) -.0694(8) .084 Uiso calc R 1 . H
C6 -.1703(3) .0656(6) -.1946(8) .063(2) Uani d . 1 . C
H6 -.1831(3) .0278(6) -.2649(8) .094 Uiso calc R 1 . H
C7 -.1833(4) .1527(6) -.2106(7) .067(2) Uani d . 1 . C
H7 -.2051(4) .1736(6) -.2907(7) .101 Uiso calc R 1 . H
C8 -.1637(3) .2110(5) -.1064(7) .053(2) Uani d . 1 . C
H8 -.1725(3) .2705(5) -.1181(7) .079 Uiso calc R 1 . H
C9 -.0734(4) -.0265(5) .1647(9) .068(2) Uani d . 1 . C
H9A -.055(2) -.0385(12) .2544(11) .102 Uiso calc R 1 . H
H9B -.048(2) -.0371(11) .117(5) .102 Uiso calc R 1 . H
H9C -.1051(4) -.0642(5) .133(6) .102 Uiso calc R 1 . H
C10 -.1369(2) .3594(4) .0879(6) .0398(13) Uani d . 1 . C
C11 -.1160(3) .4078(5) .0071(8) .058(2) Uani d . 1 . C
H11 -.0855(3) .3876(5) -.0131(8) .087 Uiso calc R 1 . H
C12 -.1415(4) .4876(6) -.0438(11) .078(3) Uani d . 1 . C
H12 -.1270(4) .5207(6) -.0965(11) .117 Uiso calc R 1 . H
C13 -.1877(3) .5184(5) -.0175(9) .070(2) Uani d . 1 . C
H13 -.2045(3) .5710(5) -.0530(9) .105 Uiso calc R 1 . H
C14 -.2083(3) .4697(5) .0618(9) .064(2) Uani d . 1 . C
H14 -.2392(3) .4897(5) .0809(9) .096 Uiso calc R 1 . H
C15 -.1832(3) .3906(5) .1142(8) .053(2) Uani d . 1 . C
H15 -.1977(3) .3582(5) .1676(8) .080 Uiso calc R 1 . H
C16 -.1432(3) .2214(4) .2567(6) .0393(13) Uani d . 1 . C
C17 -.1270(3) .2469(4) .3827(8) .049(2) Uani d . 1 . C
H17 -.0941(3) .2782(4) .4172(8) .074 Uiso calc R 1 . H
C18 -.1589(4) .2270(5) .4605(8) .056(2) Uani d . 1 . C
H18 -.1473(4) .2450(5) .5462(8) .084 Uiso calc R 1 . H
C19 -.2074(3) .1807(5) .4105(8) .055(2) Uani d . 1 . C
H19 -.2288(3) .1676(5) .4623(8) .083 Uiso calc R 1 . H
C20 -.2240(3) .1543(5) .2866(7) .051(2) Uani d . 1 . C
H20 -.2567(3) .1225(5) .2532(7) .077 Uiso calc R 1 . H
C21 -.1924(3) .1743(4) .2084(7) .0448(14) Uani d . 1 . C
H21 -.2043(3) .1560(4) .1228(7) .067 Uiso calc R 1 . H
C22 .0000 .6100(12) .2500 .052(9) Uiso d SPG .25 . C
H22A .0135(3) .5724(14) .3253(6) .079 Uiso d PGD .25 . H
Cl .0529(4) .6777(12) .2375(11) .139(7) Uani d PGD .25 . Cl
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 W C1 2 . 85.4(5) yes
C1 W C2 2 . 173.5(3) yes
C1 W C2 . . 91.7(3) yes
C1 W C2 2 2 91.7(3) yes
C1 W C2 . 2 173.5(3) yes
C2 W C2 . 2 91.8(4) yes
C1 W P 2 . 86.0(2) yes
C1 W P . . 97.3(2) yes
C2 W P . . 88.7(2) yes
C2 W P 2 . 88.3(2) yes
C1 W P 2 2 97.3(2) yes
C1 W P . 2 86.0(2) yes
C2 W P . 2 88.3(2) yes
C2 W P 2 2 88.7(2) yes
P W P . 2 175.57(7) yes
C3 P C10 . . 101.7(3) ?
C3 P C16 . . 101.3(3) ?
C10 P C16 . . 100.4(3) ?
C3 P W . . 117.4(2) ?
C10 P W . . 115.6(2) ?
C16 P W . . 117.7(2) ?
C4 O3 C9 . . 116.6(6) ?
O1 C1 W . . 175.2(7) ?
O2 C2 W . . 179.0(8) ?
C8 C3 C4 . . 116.9(6) ?
C8 C3 P . . 122.5(5) ?
C4 C3 P . . 120.5(5) ?
O3 C4 C5 . . 124.1(7) ?
O3 C4 C3 . . 114.3(6) ?
C5 C4 C3 . . 121.6(7) ?
C6 C5 C4 . . 119.0(7) ?
C6 C5 H5 . . 120.5(5) ?
C4 C5 H5 . . 120.5(5) ?
C5 C6 C7 . . 121.7(7) ?
C5 C6 H6 . . 119.2(5) ?
C7 C6 H6 . . 119.2(5) ?
C6 C7 C8 . . 120.1(8) ?
C6 C7 H7 . . 120.0(5) ?
C8 C7 H7 . . 120.0(5) ?
C3 C8 C7 . . 120.7(7) ?
C3 C8 H8 . . 119.6(4) ?
C7 C8 H8 . . 119.6(5) ?
O3 C9 H9A . . 109.5(4) ?
O3 C9 H9B . . 109.5(4) ?
H9A C9 H9B . . 109.5 ?
O3 C9 H9C . . 109.5(4) ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C11 C10 C15 . . 118.9(6) ?
C11 C10 P . . 118.0(5) ?
C15 C10 P . . 123.1(5) ?
C10 C11 C12 . . 119.2(7) ?
C10 C11 H11 . . 120.4(4) ?
C12 C11 H11 . . 120.4(5) ?
C13 C12 C11 . . 121.6(8) ?
C13 C12 H12 . . 119.2(5) ?
C11 C12 H12 . . 119.2(5) ?
C14 C13 C12 . . 118.7(7) ?
C14 C13 H13 . . 120.7(5) ?
C12 C13 H13 . . 120.7(5) ?
C13 C14 C15 . . 120.5(7) ?
C13 C14 H14 . . 119.8(5) ?
C15 C14 H14 . . 119.8(5) ?
C10 C15 C14 . . 121.1(7) ?
C10 C15 H15 . . 119.5(4) ?
C14 C15 H15 . . 119.5(5) ?
C17 C16 C21 . . 118.0(6) ?
C17 C16 P . . 120.5(5) ?
C21 C16 P . . 121.4(5) ?
C16 C17 C18 . . 121.1(7) ?
C16 C17 H17 . . 119.4(4) ?
C18 C17 H17 . . 119.4(5) ?
C19 C18 C17 . . 119.8(8) ?
C19 C18 H18 . . 120.1(5) ?
C17 C18 H18 . . 120.1(5) ?
C20 C19 C18 . . 120.1(7) ?
C20 C19 H19 . . 120.0(4) ?
C18 C19 H19 . . 120.0(5) ?
C19 C20 C21 . . 120.3(7) ?
C19 C20 H20 . . 119.8(4) ?
C21 C20 H20 . . 119.8(4) ?
C20 C21 C16 . . 120.7(7) ?
C20 C21 H21 . . 119.7(4) ?
C16 C21 H21 . . 119.7(4) ?
Cl C22 Cl . 2 107.5(3) ?
Cl C22 H22A . . 110.2 ?
Cl C22 H22A 2 . 110.5(12) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W C1 2 2.005(7) ?
W C1 . 2.005(7) yes
W C2 . 2.039(8) yes
W C2 2 2.039(8) ?
W P . 2.489(2) yes
W P 2 2.489(2) ?
P C3 . 1.828(6) ?
P C10 . 1.843(6) ?
P C16 . 1.849(7) ?
O1 C1 . 1.149(9) ?
O2 C2 . 1.152(9) ?
O3 C4 . 1.371(8) ?
O3 C9 . 1.413(8) ?
C3 C8 . 1.393(9) ?
C3 C4 . 1.415(9) ?
C4 C5 . 1.396(10) ?
C5 C6 . 1.360(12) ?
C5 H5 . .93 ?
C6 C7 . 1.361(12) ?
C6 H6 . .93 ?
C7 C8 . 1.402(10) ?
C7 H7 . .93 ?
C8 H8 . .93 ?
C9 H9A . .96 ?
C9 H9B . .96 ?
C9 H9C . .96 ?
C10 C11 . 1.385(9) ?
C10 C15 . 1.388(9) ?
C11 C12 . 1.401(11) ?
C11 H11 . .93 ?
C12 C13 . 1.385(12) ?
C12 H12 . .93 ?
C13 C14 . 1.369(12) ?
C13 H13 . .93 ?
C14 C15 . 1.393(10) ?
C14 H14 . .93 ?
C15 H15 . .93 ?
C16 C17 . 1.364(11) ?
C16 C21 . 1.391(9) ?
C17 C18 . 1.391(11) ?
C17 H17 . .93 ?
C18 C19 . 1.372(11) ?
C18 H18 . .93 ?
C19 C20 . 1.347(10) ?
C19 H19 . .93 ?
C20 C21 . 1.389(9) ?
C20 H20 . .93 ?
C21 H21 . .93 ?
C22 Cl . 1.74 ?
C22 Cl 2 1.738(12) ?
C22 H22A . .97 ?
