#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:12:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178553 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/61/4066158.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_4066158
loop_
_publ_author_name
'Bera, Holger'
'Braunschweig, Holger'
'Dörfler, Rainer'
'Kupfer, Thomas'
'Radacki, Krzysztof'
'Seeler, Fabian'
_publ_section_title
;
 Half-Sandwich Tungsten Complexes with Metal- and
 η5-Cyclopentadienyl-Bound Functional Stannyl Groups and Their
 Transformation intoAnsaComplexes†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5111
_journal_paper_doi               10.1021/om100324m
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C20 H20 O6 Sn2 W2'
_chemical_formula_sum            'C20 H20 O6 Sn2 W2'
_chemical_formula_weight         961.44
_chemical_name_common
;
?
;
_chemical_name_systematic
; 
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7023(4)
_cell_length_b                   12.7894(4)
_cell_length_c                   14.3692(5)
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.67
_cell_measurement_theta_min      2.67
_cell_volume                     2334.35(13)
_computing_cell_refinement       'Saint+ ver. 7.12A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 1.0-27 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.12A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            86374
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         33.06
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    11.970
_exptl_absorpt_correction_T_max  0.1344
_exptl_absorpt_correction_T_min  0.0924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2004/1 (Brucker Nonius 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         3.646
_refine_diff_density_min         -2.506
_refine_diff_density_rms         0.318
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         4150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0279P)²+24.6799P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                3869
_reflns_number_total             4150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100324m_si_001.cif
_cod_data_source_block           14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4066158
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-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
C1 C 0.6366(4) 0.3369(4) 0.2996(3) 0.0089(8) Uani 1 1 d .
O1 O 0.6264(3) 0.2639(3) 0.2523(3) 0.0172(7) Uani 1 1 d .
W1 W 0.650145(13) 0.467218(13) 0.372653(12) 0.00410(6) Uani 1 1 d .
C2 C 0.8014(4) 0.4379(4) 0.3509(3) 0.0101(8) Uani 1 1 d .
O2 O 0.8889(3) 0.4224(3) 0.3395(3) 0.0173(8) Uani 1 1 d .
Sn2 Sn 0.50387(2) 0.33236(2) 0.45828(2) 0.00613(7) Uani 1 1 d .
C3 C 0.7011(4) 0.4327(4) 0.4985(4) 0.0105(8) Uani 1 1 d .
O3 O 0.7346(3) 0.4176(3) 0.5723(3) 0.0156(7) Uani 1 1 d .
C4 C 0.5618(5) 0.1770(4) 0.4851(4) 0.0159(10) Uani 1 1 d .
H4A H 0.5064 0.1354 0.5148 0.024 Uiso 1 1 calc R
H4B H 0.6231 0.1808 0.5264 0.024 Uiso 1 1 calc R
H4C H 0.5824 0.1440 0.4262 0.024 Uiso 1 1 calc R
C5 C 0.3624(4) 0.3169(5) 0.3792(4) 0.0162(10) Uani 1 1 d .
H5A H 0.3141 0.2695 0.4115 0.024 Uiso 1 1 calc R
H5B H 0.3791 0.2885 0.3176 0.024 Uiso 1 1 calc R
H5C H 0.3292 0.3856 0.3723 0.024 Uiso 1 1 calc R
C11 C 0.4458(3) 0.3814(3) 0.5928(3) 0.0066(7) Uani 1 1 d .
C12 C 0.4968(4) 0.4334(4) 0.6701(3) 0.0081(8) Uani 1 1 d .
H12A H 0.5656 0.4627 0.6690 0.010 Uiso 1 1 calc R
C13 C 0.4281(4) 0.4337(4) 0.7476(3) 0.0104(8) Uani 1 1 d .
H13A H 0.4433 0.4619 0.8072 0.013 Uiso 1 1 calc R
C14 C 0.3327(4) 0.3847(4) 0.7207(3) 0.0103(8) Uani 1 1 d .
H14A H 0.2721 0.3758 0.7586 0.012 Uiso 1 1 calc R
C15 C 0.3442(4) 0.3509(4) 0.6260(3) 0.0090(9) Uani 1 1 d .
H15A H 0.2926 0.3142 0.5910 0.011 Uiso 1 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'
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'
Sn Sn -0.6537 1.4246 '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
O1 C1 W1 175.9(5) . .
C3 W1 C1 109.1(2) . .
C3 W1 C2 77.5(2) . .
C1 W1 C2 80.9(2) . .
C3 W1 C15 101.88(19) . 5_666
C1 W1 C15 148.19(19) . 5_666
C2 W1 C15 99.22(19) . 5_666
C3 W1 C14 132.79(19) . 5_666
C1 W1 C14 112.81(19) . 5_666
C2 W1 C14 88.41(19) . 5_666
C15 W1 C14 35.90(17) 5_666 5_666
C3 W1 C12 128.64(18) . 5_666
C1 W1 C12 104.42(19) . 5_666
C2 W1 C12 146.56(18) . 5_666
C15 W1 C12 58.96(17) 5_666 5_666
C14 W1 C12 58.83(17) 5_666 5_666
C3 W1 C11 99.28(18) . 5_666
C1 W1 C11 139.87(18) . 5_666
C2 W1 C11 133.98(19) . 5_666
C15 W1 C11 35.69(16) 5_666 5_666
C14 W1 C11 59.93(16) 5_666 5_666
C12 W1 C11 36.05(16) 5_666 5_666
C3 W1 C13 158.36(19) . 5_666
C1 W1 C13 91.58(19) . 5_666
C2 W1 C13 113.23(19) . 5_666
C15 W1 C13 58.87(17) 5_666 5_666
C14 W1 C13 35.18(17) 5_666 5_666
C12 W1 C13 35.00(17) 5_666 5_666
C11 W1 C13 59.50(17) 5_666 5_666
C3 W1 Sn2 71.26(14) . .
C1 W1 Sn2 70.03(14) . .
C2 W1 Sn2 126.31(14) . .
C15 W1 Sn2 128.94(12) 5_666 .
C14 W1 Sn2 144.12(13) 5_666 .
C12 W1 Sn2 85.47(12) 5_666 .
C11 W1 Sn2 94.03(11) 5_666 .
C13 W1 Sn2 111.72(13) 5_666 .
O2 C2 W1 178.8(5) . .
C5 Sn2 C4 107.3(2) . .
C5 Sn2 C11 102.4(2) . .
C4 Sn2 C11 102.96(19) . .
C5 Sn2 W1 112.30(16) . .
C4 Sn2 W1 114.67(14) . .
C11 Sn2 W1 115.97(12) . .
O3 C3 W1 176.0(4) . .
Sn2 C4 H4A 109.5 . .
Sn2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Sn2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Sn2 C5 H5A 109.5 . .
Sn2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Sn2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C15 C11 C12 105.8(4) . .
C15 C11 Sn2 121.8(3) . .
C12 C11 Sn2 131.8(3) . .
C15 C11 W1 71.6(3) . 5_666
C12 C11 W1 71.9(3) . 5_666
Sn2 C11 W1 127.4(2) . 5_666
C13 C12 C11 109.2(4) . .
C13 C12 W1 73.3(3) . 5_666
C11 C12 W1 72.0(3) . 5_666
C13 C12 H12A 125.4 . .
C11 C12 H12A 125.4 . .
W1 C12 H12A 121.0 5_666 .
C12 C13 C14 108.2(4) . .
C12 C13 W1 71.7(3) . 5_666
C14 C13 W1 71.3(3) . 5_666
C12 C13 H13A 125.9 . .
C14 C13 H13A 125.9 . .
W1 C13 H13A 122.8 5_666 .
C13 C14 C15 107.7(4) . .
C13 C14 W1 73.6(3) . 5_666
C15 C14 W1 71.9(3) . 5_666
C13 C14 H14A 126.2 . .
C15 C14 H14A 126.2 . .
W1 C14 H14A 120.2 5_666 .
C11 C15 C14 109.0(4) . .
C11 C15 W1 72.7(3) . 5_666
C14 C15 W1 72.2(3) . 5_666
C11 C15 H15A 125.5 . .
C14 C15 H15A 125.5 . .
W1 C15 H15A 121.3 5_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.162(6) .
C1 W1 1.978(5) .
W1 C3 1.971(5) .
W1 C2 1.982(5) .
W1 C15 2.327(5) 5_666
W1 C14 2.332(5) 5_666
W1 C12 2.341(5) 5_666
W1 C11 2.342(4) 5_666
W1 C13 2.362(5) 5_666
W1 Sn2 2.8180(3) .
C2 O2 1.141(6) .
Sn2 C5 2.135(5) .
Sn2 C4 2.154(5) .
Sn2 C11 2.161(5) .
C3 O3 1.159(6) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C11 C15 1.431(6) .
C11 C12 1.449(7) .
C11 W1 2.342(4) 5_666
C12 C13 1.414(7) .
C12 W1 2.341(5) 5_666
C12 H12A 0.9500 .
C13 C14 1.419(7) .
C13 W1 2.362(5) 5_666
C13 H13A 0.9500 .
C14 C15 1.436(7) .
C14 W1 2.332(5) 5_666
C14 H14A 0.9500 .
C15 W1 2.327(5) 5_666
C15 H15A 0.9500 .
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_4
C3 W1 Sn2 C5 171.1(2) . .
C1 W1 Sn2 C5 -69.5(2) . .
C2 W1 Sn2 C5 -131.1(2) . .
C15 W1 Sn2 C5 80.8(2) 5_666 .
C14 W1 Sn2 C5 32.1(3) 5_666 .
C12 W1 Sn2 C5 37.6(2) 5_666 .
C11 W1 Sn2 C5 72.7(2) 5_666 .
C13 W1 Sn2 C5 14.0(2) 5_666 .
C3 W1 Sn2 C4 -66.1(2) . .
C1 W1 Sn2 C4 53.3(2) . .
C2 W1 Sn2 C4 -8.3(3) . .
C15 W1 Sn2 C4 -156.4(2) 5_666 .
C14 W1 Sn2 C4 154.9(3) 5_666 .
C12 W1 Sn2 C4 160.4(2) 5_666 .
C11 W1 Sn2 C4 -164.5(2) 5_666 .
C13 W1 Sn2 C4 136.8(2) 5_666 .
C3 W1 Sn2 C11 53.8(2) . .
C1 W1 Sn2 C11 173.2(2) . .
C2 W1 Sn2 C11 111.6(2) . .
C15 W1 Sn2 C11 -36.5(2) 5_666 .
C14 W1 Sn2 C11 -85.2(2) 5_666 .
C12 W1 Sn2 C11 -79.71(18) 5_666 .
C11 W1 Sn2 C11 -44.7(2) 5_666 .
C13 W1 Sn2 C11 -103.34(19) 5_666 .
C5 Sn2 C11 C15 29.7(4) . .
C4 Sn2 C11 C15 -81.6(4) . .
W1 Sn2 C11 C15 152.3(3) . .
C5 Sn2 C11 C12 -160.0(4) . .
C4 Sn2 C11 C12 88.8(5) . .
W1 Sn2 C11 C12 -37.3(5) . .
C5 Sn2 C11 W1 -60.7(3) . 5_666
C4 Sn2 C11 W1 -172.0(3) . 5_666
W1 Sn2 C11 W1 61.9(3) . 5_666
C15 C11 C12 C13 0.3(5) . .
Sn2 C11 C12 C13 -171.2(3) . .
W1 C11 C12 C13 64.4(3) 5_666 .
C15 C11 C12 W1 -64.1(3) . 5_666
Sn2 C11 C12 W1 124.4(4) . 5_666
C11 C12 C13 C14 -1.2(5) . .
W1 C12 C13 C14 62.3(3) 5_666 .
C11 C12 C13 W1 -63.5(3) . 5_666
C12 C13 C14 C15 1.7(5) . .
W1 C13 C14 C15 64.3(3) 5_666 .
C12 C13 C14 W1 -62.6(3) . 5_666
C12 C11 C15 C14 0.8(5) . .
Sn2 C11 C15 C14 173.3(3) . .
W1 C11 C15 C14 -63.5(3) 5_666 .
C12 C11 C15 W1 64.3(3) . 5_666
Sn2 C11 C15 W1 -123.1(3) . 5_666
C13 C14 C15 C11 -1.5(5) . .
W1 C14 C15 C11 63.8(3) 5_666 .
C13 C14 C15 W1 -65.4(3) . 5_666
