#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314108.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_4314108
loop_
_publ_author_name
'Berthold Hoge'
'Tobias Herrmann'
'Christoph Thösen'
'Ingo Pantenburg'
_publ_section_title
;
 Preparation and Characterization of [Hg{P(C6F5)2}2],
 [Hg{(μ-P(C6F5)2)W(CO)5}2], and [Hg{(μ-P(CF3)2)W(CO)5}2] and the X-ray
 Crystal Structure of [Hg{(μ-P(C6F5)2)W(CO)5}2].2DMF
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5422
_journal_page_last               5428
_journal_paper_doi               10.1021/ic034448n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C40 H14 F20 Hg N2 O12 P2 W2'
_chemical_formula_weight         1724.76
_chemical_name_systematic
;
 ?
;
_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'
_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                 104.011(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.662(3)
_cell_length_b                   10.4691(10)
_cell_length_c                   20.264(3)
_cell_measurement_temperature    170(2)
_cell_volume                     4870.5(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      293(2)
_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  0.1030
_diffrn_reflns_av_sigmaI/netI    0.1143
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22263
_diffrn_reflns_theta_max         27.32
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    8.061
_exptl_absorpt_correction_T_max  0.4306
_exptl_absorpt_correction_T_min  0.2552
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    2.352
_exptl_crystal_F_000             3208
_refine_diff_density_max         1.173
_refine_diff_density_min         -2.050
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       0.000048(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.800
_refine_ls_goodness_of_fit_obs   0.939
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_restrained_S_obs      0.939
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_obs          0.0370
_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)+(0.0027P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0493
_refine_ls_wR_factor_obs         0.0428
_reflns_number_observed          3139
_reflns_number_total             5408
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034448nsi20030429_071238.cif
_cod_data_source_block           bhhgw
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0027P)^2^+0.0000P] 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^)+(0.0027P)^2^+0.0000P] 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               4314108
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_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
Hg1 Hg 0.5000 0.68796(4) 0.2500 0.02502(12) Uani 1 d S .
W2 W 0.62197(2) 0.53465(3) 0.149093(14) 0.03003(9) Uani 1 d . .
C1 C 0.5524(4) 0.6046(8) 0.0822(3) 0.044(2) Uani 1 d . .
O1 O 0.5119(3) 0.6444(6) 0.0405(3) 0.064(2) Uani 1 d . .
C2 C 0.6327(4) 0.4174(8) 0.0758(4) 0.046(2) Uani 1 d . .
O2 O 0.6381(3) 0.3471(6) 0.0338(3) 0.069(2) Uani 1 d . .
C3 C 0.5745(4) 0.3998(7) 0.1840(3) 0.034(2) Uani 1 d . .
O3 O 0.5475(3) 0.3261(6) 0.2059(3) 0.051(2) Uani 1 d . .
C4 C 0.6940(4) 0.4604(8) 0.2096(3) 0.038(2) Uani 1 d . .
O4 O 0.7372(3) 0.4162(6) 0.2429(3) 0.048(2) Uani 1 d . .
C5 C 0.6740(4) 0.6725(8) 0.1229(3) 0.039(2) Uani 1 d . .
O5 O 0.7051(3) 0.7485(6) 0.1105(3) 0.055(2) Uani 1 d . .
P1 P 0.60191(8) 0.6681(2) 0.24582(7) 0.0238(4) Uani 1 d . .
C11 C 0.6413(3) 0.5892(7) 0.3251(3) 0.027(2) Uani 1 d . .
C12 C 0.7007(3) 0.5995(7) 0.3476(3) 0.032(2) Uani 1 d . .
F12 F 0.7305(2) 0.6755(5) 0.3137(2) 0.0435(11) Uani 1 d . .
C13 C 0.7330(3) 0.5328(9) 0.4025(3) 0.038(2) Uani 1 d . .
F13 F 0.7905(2) 0.5468(5) 0.4218(2) 0.0558(13) Uani 1 d . .
C14 C 0.7050(3) 0.4525(7) 0.4385(3) 0.033(2) Uani 1 d . .
F14 F 0.7355(2) 0.3878(5) 0.4924(2) 0.0537(14) Uani 1 d . .
C15 C 0.6454(4) 0.4410(7) 0.4180(3) 0.034(2) Uani 1 d . .
F15 F 0.6179(2) 0.3636(4) 0.4533(2) 0.0503(13) Uani 1 d . .
C16 C 0.6147(4) 0.5090(7) 0.3623(3) 0.032(2) Uani 1 d . .
F16 F 0.5562(2) 0.4904(4) 0.3462(2) 0.0425(12) Uani 1 d . .
C21 C 0.6250(3) 0.8366(7) 0.2597(3) 0.023(2) Uani 1 d . .
C22 C 0.6458(3) 0.8959(8) 0.3225(3) 0.030(2) Uani 1 d . .
F22 F 0.6526(2) 0.8285(4) 0.3810(2) 0.0410(12) Uani 1 d . .
C23 C 0.6584(3) 1.0233(9) 0.3304(3) 0.035(2) Uani 1 d . .
F23 F 0.6774(2) 1.0744(4) 0.3927(2) 0.0524(14) Uani 1 d . .
C24 C 0.6521(4) 1.0992(7) 0.2744(4) 0.036(2) Uani 1 d . .
F24 F 0.6639(2) 1.2247(4) 0.2817(2) 0.0554(14) Uani 1 d . .
C25 C 0.6307(3) 1.0473(8) 0.2104(3) 0.032(2) Uani 1 d . .
F25 F 0.6243(2) 1.1210(4) 0.1549(2) 0.0465(12) Uani 1 d . .
C26 C 0.6183(3) 0.9199(7) 0.2040(3) 0.030(2) Uani 1 d . .
F26 F 0.5987(2) 0.8734(4) 0.1406(2) 0.0375(12) Uani 1 d . .
O6 O 0.5154(3) 0.8710(7) 0.3357(3) 0.074(2) Uani 1 d . .
C7 C 0.5383(5) 0.8930(11) 0.3943(5) 0.057(3) Uani 1 d . .
H7 H 0.5501(5) 0.8230(11) 0.4225(5) 0.089(40) Uiso 1 calc R .
N8 N 0.5482(3) 1.0062(6) 0.4221(3) 0.039(2) Uani 1 d . .
C81 C 0.5794(5) 1.0258(13) 0.4925(4) 0.088(4) Uani 1 d . .
H81A H 0.5818(5) 1.1156(13) 0.5024(4) 0.239(34) Uiso 1 calc R .
H81B H 0.6180(5) 0.9911(13) 0.4997(4) 0.239(34) Uiso 1 calc R .
H81C H 0.5591(5) 0.9836(13) 0.5220(4) 0.239(34) Uiso 1 calc R .
C82 C 0.5289(5) 1.1211(10) 0.3827(5) 0.075(3) Uani 1 d . .
H82A H 0.5398(5) 1.1948(10) 0.4111(5) 0.239(34) Uiso 1 calc R .
H82B H 0.4873(5) 1.1190(10) 0.3660(5) 0.239(34) Uiso 1 calc R .
H82C H 0.5468(5) 1.1252(10) 0.3450(5) 0.239(34) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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'
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
P1 Hg1 P1 170.25(9) . 2_655 ?
P1 Hg1 O6 91.1(2) . 2_655 ?
P1 Hg1 O6 96.2(2) 2_655 2_655 ?
P1 Hg1 O6 96.2(2) . . ?
P1 Hg1 O6 91.1(2) 2_655 . ?
O6 Hg1 O6 82.7(3) 2_655 . ?
C2 W2 C4 88.5(3) . . ?
C2 W2 C1 87.3(3) . . ?
C4 W2 C1 175.4(3) . . ?
C2 W2 C3 90.7(3) . . ?
C4 W2 C3 88.7(3) . . ?
C1 W2 C3 93.2(3) . . ?
C2 W2 C5 92.7(3) . . ?
C4 W2 C5 87.5(3) . . ?
C1 W2 C5 90.8(3) . . ?
C3 W2 C5 174.8(3) . . ?
C2 W2 P1 174.5(3) . . ?
C4 W2 P1 91.8(2) . . ?
C1 W2 P1 92.6(2) . . ?
C3 W2 P1 83.8(2) . . ?
C5 W2 P1 92.8(2) . . ?
O1 C1 W2 177.5(6) . . ?
O2 C2 W2 178.3(8) . . ?
O3 C3 W2 177.5(6) . . ?
O4 C4 W2 177.4(6) . . ?
O5 C5 W2 177.1(7) . . ?
C11 P1 C21 103.1(3) . . ?
C11 P1 Hg1 107.6(2) . . ?
C21 P1 Hg1 99.9(2) . . ?
C11 P1 W2 106.0(2) . . ?
C21 P1 W2 122.6(2) . . ?
Hg1 P1 W2 116.33(7) . . ?
C12 C11 C16 115.7(6) . . ?
C12 C11 P1 120.9(5) . . ?
C16 C11 P1 123.2(6) . . ?
F12 C12 C11 119.7(6) . . ?
F12 C12 C13 116.8(7) . . ?
C11 C12 C13 123.5(7) . . ?
F13 C13 C12 120.7(7) . . ?
F13 C13 C14 119.9(6) . . ?
C12 C13 C14 119.4(7) . . ?
F14 C14 C15 120.9(7) . . ?
F14 C14 C13 120.4(7) . . ?
C15 C14 C13 118.7(6) . . ?
F15 C15 C14 118.9(6) . . ?
F15 C15 C16 121.0(7) . . ?
C14 C15 C16 120.1(7) . . ?
F16 C16 C11 122.0(6) . . ?
F16 C16 C15 115.3(7) . . ?
C11 C16 C15 122.7(8) . . ?
C22 C21 C26 113.8(6) . . ?
C22 C21 P1 126.2(5) . . ?
C26 C21 P1 119.9(5) . . ?
F22 C22 C23 115.4(6) . . ?
F22 C22 C21 120.5(7) . . ?
C23 C22 C21 124.1(7) . . ?
F23 C23 C24 119.7(8) . . ?
F23 C23 C22 120.8(7) . . ?
C24 C23 C22 119.6(7) . . ?
F24 C24 C23 120.1(7) . . ?
F24 C24 C25 120.3(7) . . ?
C23 C24 C25 119.6(7) . . ?
F25 C25 C26 120.3(6) . . ?
F25 C25 C24 120.1(7) . . ?
C26 C25 C24 119.6(6) . . ?
F26 C26 C25 117.4(6) . . ?
F26 C26 C21 119.2(6) . . ?
C25 C26 C21 123.4(6) . . ?
C7 O6 Hg1 140.5(7) . . ?
O6 C7 N8 126.1(11) . . ?
C7 N8 C81 123.1(9) . . ?
C7 N8 C82 120.9(8) . . ?
C81 N8 C82 116.0(8) . . ?
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
Hg1 P1 2.442(2) . ?
Hg1 P1 2.442(2) 2_655 ?
Hg1 O6 2.553(6) 2_655 ?
Hg1 O6 2.553(6) . ?
W2 C2 1.990(9) . ?
W2 C4 2.001(9) . ?
W2 C1 2.002(9) . ?
W2 C3 2.036(9) . ?
W2 C5 2.049(9) . ?
W2 P1 2.544(2) . ?
C1 O1 1.188(9) . ?
C2 O2 1.155(9) . ?
C3 O3 1.156(8) . ?
C4 O4 1.174(9) . ?
C5 O5 1.152(9) . ?
P1 C11 1.845(7) . ?
P1 C21 1.847(7) . ?
C11 C12 1.373(10) . ?
C11 C16 1.379(10) . ?
C12 F12 1.356(8) . ?
C12 C13 1.379(10) . ?
C13 F13 1.330(8) . ?
C13 C14 1.382(10) . ?
C14 F14 1.339(7) . ?
C14 C15 1.375(10) . ?
C15 F15 1.350(8) . ?
C15 C16 1.382(9) . ?
C16 F16 1.355(8) . ?
C21 C22 1.394(8) . ?
C21 C26 1.405(9) . ?
C22 F22 1.355(7) . ?
C22 C23 1.368(10) . ?
C23 F23 1.344(8) . ?
C23 C24 1.362(10) . ?
C24 F24 1.344(8) . ?
C24 C25 1.385(10) . ?
C25 F25 1.341(7) . ?
C25 C26 1.366(10) . ?
C26 F26 1.345(7) . ?
O6 C7 1.202(10) . ?
C7 N8 1.308(10) . ?
N8 C81 1.454(9) . ?
N8 C82 1.455(11) . ?
