#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:17:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179916 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/11/7021113.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_7021113
loop_
_publ_author_name
'Dolci, Sara'
'Marchetti, Fabio'
'Pampaloni, Guido'
'Zacchini, Stefano'
_publ_section_title
;
 A crystallographic and spectroscopic study on the reactions of WCl6 with
 carbonyl compounds.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5635
_journal_page_last               5648
_journal_paper_doi               10.1039/c2dt32771f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C3 H5 Cl4 O3 W'
_chemical_formula_weight         414.72
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.147(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.305(4)
_cell_length_b                   9.7756(19)
_cell_length_c                   12.088(2)
_cell_measurement_reflns_used    5026
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.407
_cell_measurement_theta_min      2.4485
_cell_volume                     1870.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7541
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    13.450
_exptl_absorpt_correction_T_max  0.2547
_exptl_absorpt_correction_T_min  0.2221
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.291
_refine_diff_density_min         -2.059
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0111P)²+34.1802P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                1979
_reflns_number_total             2039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32771f.txt
_cod_data_source_block           fm2605b9_C2C
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7021113
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.3143(4) 0.2051(7) 0.2169(6) 0.0252(13) Uani 1 1 d .
H1A H 0.3454 0.2668 0.1900 0.030 Uiso 1 1 calc R
H1B H 0.3449 0.1170 0.2448 0.030 Uiso 1 1 calc R
C2 C 0.3059(4) 0.2684(6) 0.3229(6) 0.0207(12) Uani 1 1 d .
C3 C 0.3681(4) 0.3408(7) 0.5371(6) 0.0266(14) Uani 1 1 d .
H3A H 0.4243 0.3450 0.6137 0.040 Uiso 1 1 calc R
H3B H 0.3310 0.2835 0.5544 0.040 Uiso 1 1 calc R
H3C H 0.3444 0.4332 0.5141 0.040 Uiso 1 1 calc R
Cl1 Cl 0.05506(10) 0.39424(15) 0.15898(17) 0.0272(3) Uani 1 1 d .
Cl2 Cl 0.04523(12) 0.2154(2) -0.0977(2) 0.0429(4) Uani 1 1 d .
Cl3 Cl 0.17656(10) 0.46972(15) 0.04475(15) 0.0237(3) Uani 1 1 d .
Cl4 Cl 0.09852(10) 0.07128(15) 0.17467(15) 0.0246(3) Uani 1 1 d .
O1 O 0.2303(3) 0.1844(4) 0.1149(4) 0.0244(9) Uani 1 1 d .
O2 O 0.2349(2) 0.3041(4) 0.3002(4) 0.0184(8) Uani 1 1 d .
O3 O 0.3747(3) 0.2819(4) 0.4312(4) 0.0234(9) Uani 1 1 d .
W1 W 0.134588(16) 0.26539(2) 0.10061(3) 0.02179(9) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.025(3) 0.027(3) 0.035(4) 0.003(3) 0.023(3) 0.006(3)
C2 0.018(3) 0.013(3) 0.033(3) 0.007(2) 0.014(3) 0.001(2)
C3 0.022(3) 0.032(3) 0.029(3) 0.000(3) 0.015(3) -0.001(3)
Cl1 0.0254(7) 0.0199(7) 0.0489(10) -0.0040(6) 0.0280(7) -0.0002(6)
Cl2 0.0366(10) 0.0517(11) 0.0480(11) -0.0089(9) 0.0268(9) -0.0081(8)
Cl3 0.0264(7) 0.0201(7) 0.0317(8) 0.0018(6) 0.0198(7) -0.0011(6)
Cl4 0.0276(8) 0.0172(7) 0.0354(8) -0.0028(6) 0.0205(7) -0.0035(6)
O1 0.025(2) 0.019(2) 0.039(3) -0.0013(19) 0.024(2) 0.0020(17)
O2 0.018(2) 0.020(2) 0.023(2) -0.0025(16) 0.0147(18) -0.0010(16)
O3 0.019(2) 0.024(2) 0.033(2) 0.0063(18) 0.017(2) 0.0045(17)
W1 0.02226(14) 0.01606(13) 0.03662(15) -0.00223(10) 0.02190(11) -0.00033(9)
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'
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
O1 C1 C2 105.6(5)
O1 C1 H1A 110.6
C2 C1 H1A 110.6
O1 C1 H1B 110.6
C2 C1 H1B 110.6
H1A C1 H1B 108.7
O2 C2 O3 125.4(6)
O2 C2 C1 118.3(6)
O3 C2 C1 116.3(5)
O3 C3 H3A 109.5
O3 C3 H3B 109.5
H3A C3 H3B 109.5
O3 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
C1 O1 W1 125.5(4)
C2 O2 W1 113.5(4)
C2 O3 C3 117.4(5)
O1 W1 Cl2 99.20(15)
O1 W1 O2 75.09(17)
Cl2 W1 O2 174.27(11)
O1 W1 Cl1 157.86(15)
Cl2 W1 Cl1 102.75(7)
O2 W1 Cl1 82.97(11)
O1 W1 Cl4 93.04(14)
Cl2 W1 Cl4 92.25(7)
O2 W1 Cl4 87.74(11)
Cl1 W1 Cl4 89.02(5)
O1 W1 Cl3 87.72(14)
Cl2 W1 Cl3 92.72(7)
O2 W1 Cl3 87.47(11)
Cl1 W1 Cl3 88.35(5)
Cl4 W1 Cl3 174.78(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.422(8)
C1 C2 1.499(9)
C1 H1A 0.9900
C1 H1B 0.9900
C2 O2 1.236(7)
C2 O3 1.289(8)
C3 O3 1.464(8)
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
Cl1 W1 2.2881(14)
Cl2 W1 2.173(2)
Cl3 W1 2.3574(15)
Cl4 W1 2.3306(15)
O1 W1 1.849(4)
O2 W1 2.211(4)
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
O1 C1 C2 O2 -8.2(7)
O1 C1 C2 O3 172.3(5)
C2 C1 O1 W1 16.3(7)
O3 C2 O2 W1 179.0(4)
C1 C2 O2 W1 -0.5(6)
O2 C2 O3 C3 1.8(8)
C1 C2 O3 C3 -178.8(5)
C1 O1 W1 Cl2 167.0(4)
C1 O1 W1 O2 -13.4(4)
C1 O1 W1 Cl1 -5.3(7)
C1 O1 W1 Cl4 -100.2(5)
C1 O1 W1 Cl3 74.6(5)
C2 O2 W1 O1 6.9(4)
C2 O2 W1 Cl2 10.7(14)
C2 O2 W1 Cl1 -170.0(4)
C2 O2 W1 Cl4 100.7(4)
C2 O2 W1 Cl3 -81.4(4)
