#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:17:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179916 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/11/7021117.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_7021117
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 H7 Cl4 N O2 W'
_chemical_formula_weight         414.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   6.3608(4)
_cell_length_b                   9.9793(7)
_cell_length_c                   16.0433(11)
_cell_measurement_reflns_used    5121
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.667
_cell_measurement_theta_min      2.4035
_cell_volume                     1018.37(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7238
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    12.347
_exptl_absorpt_correction_T_max  0.3437
_exptl_absorpt_correction_T_min  0.2427
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.619(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0166
_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)+(0.0188P)²+0.4556P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0383
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                2320
_reflns_number_total             2384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32771f.txt
_cod_data_source_block           fm250509_P2121
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7021117
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'
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 0.7995(7) 0.8946(4) 0.7229(3) 0.0151(9) Uani 1 1 d D
H1 H 0.692(5) 0.870(4) 0.759(2) 0.018 Uiso 1 1 d D
C2 C 0.9024(7) 0.9551(4) 0.5827(2) 0.0195(9) Uani 1 1 d .
H2A H 0.8341 0.9612 0.5281 0.029 Uiso 1 1 calc R
H2B H 1.0186 0.8908 0.5799 0.029 Uiso 1 1 calc R
H2C H 0.9568 1.0433 0.5986 0.029 Uiso 1 1 calc R
C3 C 0.5346(7) 0.8868(5) 0.6166(3) 0.0248(11) Uani 1 1 d .
H3A H 0.5261 0.9041 0.5566 0.037 Uiso 1 1 calc R
H3B H 0.4385 0.9471 0.6462 0.037 Uiso 1 1 calc R
H3C H 0.4949 0.7937 0.6279 0.037 Uiso 1 1 calc R
Cl1 Cl 0.89908(16) 1.12214(10) 0.87875(7) 0.0201(2) Uani 1 1 d .
Cl2 Cl 0.85286(17) 0.80245(11) 0.91699(7) 0.0207(2) Uani 1 1 d .
Cl3 Cl 1.31450(15) 0.75088(11) 0.83449(7) 0.0190(2) Uani 1 1 d .
Cl4 Cl 1.35874(16) 1.06951(10) 0.79698(7) 0.0216(2) Uani 1 1 d .
N1 N 0.7485(5) 0.9100(3) 0.6452(2) 0.0139(8) Uani 1 1 d .
O1 O 0.9845(4) 0.9124(3) 0.7493(2) 0.0156(6) Uani 1 1 d .
O2 O 1.2332(5) 0.9621(3) 0.9658(2) 0.0240(8) Uani 1 1 d .
W1 W 1.12341(2) 0.938558(15) 0.870907(9) 0.01265(5) 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 0.019(2) 0.0098(19) 0.017(2) -0.0009(17) 0.0025(17) 0.0000(15)
C2 0.023(2) 0.020(2) 0.0153(19) 0.0022(17) 0.0024(17) 0.001(2)
C3 0.018(2) 0.034(3) 0.023(3) 0.002(2) -0.005(2) -0.0011(19)
Cl1 0.0198(5) 0.0174(4) 0.0232(5) -0.0005(4) 0.0014(5) 0.0054(4)
Cl2 0.0186(5) 0.0220(5) 0.0216(5) 0.0038(4) 0.0047(5) -0.0017(5)
Cl3 0.0184(5) 0.0149(5) 0.0237(5) 0.0001(4) 0.0042(4) 0.0026(4)
Cl4 0.0167(4) 0.0160(4) 0.0320(5) 0.0021(4) 0.0033(4) -0.0046(5)
N1 0.0136(15) 0.0121(18) 0.016(2) -0.0014(14) -0.0011(13) -0.0013(13)
O1 0.0142(13) 0.0183(17) 0.0142(15) 0.0001(12) 0.0010(11) -0.0010(12)
O2 0.0241(15) 0.029(2) 0.0189(16) -0.0051(15) -0.0066(13) 0.0034(14)
W1 0.01231(7) 0.01326(7) 0.01237(7) -0.00080(6) -0.00080(7) 0.00069(7)
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'
N N 0.0061 0.0033 '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 N1 122.6(4)
O1 C1 H1 121(3)
N1 C1 H1 117(3)
N1 C2 H2A 109.5
N1 C2 H2B 109.5
H2A C2 H2B 109.5
N1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
N1 C3 H3A 109.5
N1 C3 H3B 109.5
H3A C3 H3B 109.5
N1 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
C1 N1 C3 121.2(4)
C1 N1 C2 121.6(4)
C3 N1 C2 117.1(4)
C1 O1 W1 134.6(3)
O2 W1 O1 178.93(15)
O2 W1 Cl3 97.06(11)
O1 W1 Cl3 83.61(9)
O2 W1 Cl2 95.80(12)
O1 W1 Cl2 85.02(8)
Cl3 W1 Cl2 89.78(4)
O2 W1 Cl4 96.64(12)
O1 W1 Cl4 82.53(8)
Cl3 W1 Cl4 89.30(4)
Cl2 W1 Cl4 167.54(4)
O2 W1 Cl1 95.48(11)
O1 W1 Cl1 83.84(8)
Cl3 W1 Cl1 167.45(4)
Cl2 W1 Cl1 89.36(4)
Cl4 W1 Cl1 88.84(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.263(5)
C1 N1 1.297(6)
C1 H1 0.931(10)
C2 N1 1.471(5)
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 N1 1.455(5)
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
Cl1 W1 2.3256(10)
Cl2 W1 2.3136(11)
Cl3 W1 2.3079(10)
Cl4 W1 2.3141(10)
O1 W1 2.157(3)
O2 W1 1.691(3)
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 N1 C3 179.2(4)
O1 C1 N1 C2 -2.6(7)
N1 C1 O1 W1 164.7(3)
C1 O1 W1 O2 -110(7)
C1 O1 W1 Cl3 121.5(4)
C1 O1 W1 Cl2 31.1(4)
C1 O1 W1 Cl4 -148.4(4)
C1 O1 W1 Cl1 -58.8(4)
