#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008211.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_7008211
loop_
_publ_author_name
'Crause, Chantelle'
'Görls, Helmar'
'Lotz, Simon'
_publ_section_title
;
 Binuclear biscarbene complexes of furan.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1649
_journal_page_last               1657
_journal_paper_doi               10.1039/b419148j
_journal_year                    2005
_chemical_formula_sum            'C20 H12 O13 W2'
_chemical_formula_weight         828.00
_chemical_melting_point          'decompose on heating'
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.435(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8784(9)
_cell_length_b                   7.6038(3)
_cell_length_c                   13.3500(6)
_cell_measurement_temperature    183(2)
_cell_volume                     2403.53(17)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '(phi- + omega-scan)'
_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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9142
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    9.629
_exptl_absorpt_correction_T_max  0.286
_exptl_absorpt_correction_T_min  0.197
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.772
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0599
_reflns_number_gt                2283
_reflns_number_total             2775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419148j.txt
_cod_data_source_block           FO1427
_cod_original_cell_volume        2403.5(2)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7008211
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.126925(9) 0.0000 0.319377(17) 0.02644(8) Uani 1 2 d S . .
W2 W 0.429868(9) 0.0000 0.170884(17) 0.02810(8) Uani 1 2 d S . .
O1 O 0.26607(15) 0.0000 0.3010(3) 0.0275(9) Uani 1 2 d S . .
O2 O 0.21000(16) 0.0000 0.5279(3) 0.0327(10) Uani 1 2 d S . .
O3 O 0.29439(17) 0.0000 0.1296(3) 0.0345(10) Uani 1 2 d S . .
O4 O 0.18282(13) 0.2870(5) 0.1891(3) 0.0538(9) Uani 1 1 d . . .
O5 O 0.01680(19) 0.0000 0.1561(3) 0.0467(12) Uani 1 2 d S . .
O6 O 0.06510(14) 0.2994(5) 0.4302(3) 0.0548(9) Uani 1 1 d . . .
O7 O 0.41714(16) -0.2948(5) -0.0005(3) 0.0632(11) Uani 1 1 d . . .
O8 O 0.5627(2) 0.0000 0.1682(4) 0.0626(15) Uani 1 2 d S . .
O9 O 0.44916(14) 0.3030(4) 0.3353(3) 0.0485(9) Uani 1 1 d . . .
C1 C 0.3419(3) 0.0000 0.1948(4) 0.0287(13) Uani 1 2 d S . .
C2 C 0.3238(2) 0.0000 0.2943(4) 0.0289(13) Uani 1 2 d S . .
C3 C 0.3528(2) 0.0000 0.3908(4) 0.0319(14) Uani 1 2 d S . .
H3A H 0.3926 0.0000 0.4086 0.038 Uiso 1 2 calc SR . .
C4 C 0.3116(2) 0.0000 0.4581(4) 0.0321(14) Uani 1 2 d S . .
H4A H 0.3188 0.0000 0.5297 0.039 Uiso 1 2 calc SR . .
C5 C 0.2597(2) 0.0000 0.4014(4) 0.0277(13) Uani 1 2 d S . .
C6 C 0.2018(2) 0.0000 0.4265(4) 0.0269(12) Uani 1 2 d S . .
C7 C 0.1616(2) 0.0000 0.5856(4) 0.0353(15) Uani 1 2 d S . .
H7A H 0.1380 -0.1057 0.5692 0.042 Uiso 0.50 1 calc PR . .
H7B H 0.1380 0.1057 0.5692 0.042 Uiso 0.50 1 calc PR . .
C8 C 0.1854(3) 0.0000 0.6950(4) 0.0407(16) Uani 1 2 d S . .
H8A H 0.1545 0.0000 0.7366 0.061 Uiso 1 2 calc SR . .
H8B H 0.2087 0.1052 0.7101 0.061 Uiso 0.50 1 calc PR . .
H8C H 0.2087 -0.1052 0.7100 0.061 Uiso 0.50 1 calc PR . .
C9 C 0.2967(3) 0.0000 0.0210(4) 0.0387(16) Uani 1 2 d S . .
H9A H 0.3166 -0.1059 0.0007 0.046 Uiso 0.50 1 calc PR . .
H9B H 0.3166 0.1059 0.0007 0.046 Uiso 0.50 1 calc PR . .
C10 C 0.2352(3) 0.0000 -0.0276(5) 0.0454(18) Uani 1 2 d S . .
H10A H 0.2338 0.0000 -0.1013 0.068 Uiso 1 2 calc SR . .
H10B H 0.2162 0.1052 -0.0063 0.068 Uiso 0.50 1 calc PR . .
H10C H 0.2162 -0.1052 -0.0063 0.068 Uiso 0.50 1 calc PR . .
C11 C 0.16293(18) 0.1847(6) 0.2370(3) 0.0366(10) Uani 1 1 d . . .
C12 C 0.0569(3) 0.0000 0.2134(5) 0.0332(14) Uani 1 2 d S . .
C13 C 0.08823(17) 0.1897(6) 0.3928(3) 0.0353(10) Uani 1 1 d . . .
C14 C 0.42006(19) -0.1919(6) 0.0598(4) 0.0400(11) Uani 1 1 d . . .
C15 C 0.5151(3) 0.0000 0.1658(5) 0.0398(16) Uani 1 2 d S . .
C16 C 0.44226(16) 0.1924(6) 0.2770(3) 0.0325(10) Uani 1 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'
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
C13 W1 C13 90.5(3) . 6 ?
C13 W1 C11 91.21(19) . . ?
C13 W1 C11 176.22(16) 6 . ?
C13 W1 C11 176.23(16) . 6 ?
C13 W1 C11 91.20(19) 6 6 ?
C11 W1 C11 86.9(2) . 6 ?
C13 W1 C12 87.22(16) . . ?
C13 W1 C12 87.22(16) 6 . ?
C11 W1 C12 89.47(16) . . ?
C11 W1 C12 89.47(16) 6 . ?
C13 W1 C6 94.03(15) . . ?
C13 W1 C6 94.04(15) 6 . ?
C11 W1 C6 89.23(16) . . ?
C11 W1 C6 89.23(16) 6 . ?
C12 W1 C6 178.21(19) . . ?
C16 W2 C16 92.1(2) 6 . ?
C16 W2 C15 88.13(16) 6 . ?
C16 W2 C15 88.13(16) . . ?
C16 W2 C14 177.56(15) 6 6 ?
C16 W2 C14 89.12(18) . 6 ?
C15 W2 C14 89.83(18) . 6 ?
C16 W2 C14 89.12(18) 6 . ?
C16 W2 C14 177.56(15) . . ?
C15 W2 C14 89.83(18) . . ?
C14 W2 C14 89.5(2) 6 . ?
C16 W2 C1 87.35(15) 6 . ?
C16 W2 C1 87.35(15) . . ?
C15 W2 C1 173.5(2) . . ?
C14 W2 C1 94.79(16) 6 . ?
C14 W2 C1 94.79(16) . . ?
C5 O1 C2 107.4(4) . . ?
C6 O2 C7 120.4(5) . . ?
C1 O3 C9 120.7(4) . . ?
O3 C1 C2 105.6(5) . . ?
O3 C1 W2 131.4(4) . . ?
C2 C1 W2 123.0(4) . . ?
C3 C2 O1 108.7(5) . . ?
C3 C2 C1 133.1(5) . . ?
O1 C2 C1 118.2(5) . . ?
C2 C3 C4 106.7(5) . . ?
C5 C4 C3 107.7(5) . . ?
C4 C5 O1 109.5(5) . . ?
C4 C5 C6 133.7(5) . . ?
O1 C5 C6 116.9(5) . . ?
O2 C6 C5 102.2(5) . . ?
O2 C6 W1 132.4(4) . . ?
C5 C6 W1 125.4(4) . . ?
O2 C7 C8 106.6(5) . . ?
O3 C9 C10 105.4(5) . . ?
O4 C11 W1 178.8(4) . . ?
O5 C12 W1 178.1(5) . . ?
O6 C13 W1 176.9(4) . . ?
O7 C14 W2 177.0(4) . . ?
O8 C15 W2 176.5(6) . . ?
O9 C16 W2 178.7(4) . . ?
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 C13 2.032(4) . ?
W1 C13 2.032(4) 6 ?
W1 C11 2.041(5) . ?
W1 C11 2.041(5) 6 ?
W1 C12 2.046(7) . ?
W1 C6 2.139(6) . ?
W2 C16 2.031(4) 6 ?
W2 C16 2.031(4) . ?
W2 C15 2.044(7) . ?
W2 C14 2.072(5) 6 ?
W2 C14 2.072(5) . ?
W2 C1 2.166(6) . ?
O1 C5 1.370(6) . ?
O1 C2 1.393(6) . ?
O2 C6 1.343(6) . ?
O2 C7 1.470(6) . ?
O3 C1 1.337(7) . ?
O3 C9 1.458(6) . ?
O4 C11 1.147(5) . ?
O5 C12 1.145(7) . ?
O6 C13 1.149(5) . ?
O7 C14 1.118(5) . ?
O8 C15 1.133(7) . ?
O9 C16 1.144(5) . ?
C1 C2 1.448(8) . ?
C2 C3 1.382(8) . ?
C3 C4 1.414(7) . ?
C4 C5 1.366(8) . ?
C5 C6 1.464(7) . ?
C7 C8 1.498(8) . ?
C9 C10 1.525(9) . ?
