#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/38/4113830.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_4113830
loop_
_publ_author_name
'Christian Cremer'
'Peter Burger'
_publ_contact_author_address
; 
'Anorg.-Chem Inst., University of Zuerich, Winterthurerstr. 190, 8057 Zuerich'
;
_publ_contact_author_email       chburger@aci.unizh.ch
_publ_contact_author_fax         '+41 1 635 6802'
_publ_contact_author_name        'Peter Burger*'
_publ_contact_author_phone       '+41 1 635 4692'
_publ_section_title
;
 Magnetic Properties of Cationic Tungsten(IV) Half Sandwich Compounds:
 Experimental and Theoretical Study of a Solvent and Ligand Stabilized
 Singlet Ground State Leading to a Thermally Induced Singlet-Triplet Spin
 State Interconversion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7664
_journal_page_last               7677
_journal_paper_doi               10.1021/ja028313c
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        synthesis
_chemical_formula_sum            'C24 H32 Cl2 N2 O0.5 W'
_chemical_formula_weight         611.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                102.84(3)
_cell_angle_beta                 101.01(3)
_cell_angle_gamma                101.60(3)
_cell_formula_units_Z            2
_cell_length_a                   8.369(2)
_cell_length_b                   10.952(2)
_cell_length_c                   13.977(3)
_cell_measurement_temperature    183(2)
_cell_volume                     1185.7(5)
_computing_cell_refinement       'Stoe IPDS software'
_computing_data_collection       'Stoe IPDS software'
_computing_data_reduction        'Stoe IPDS software'
_computing_molecular_graphics    'Ortep32   (Farrugia, 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       'Image Plate'
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10705
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    5.112
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       'rect. parallelepiped'
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.156
_refine_diff_density_min         -1.442
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4177
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.045
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_obs          0.0318
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0569P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0814
_refine_ls_wR_factor_obs         0.0776
_reflns_number_observed          3695
_reflns_number_total             4179
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja028313c_2.cif
_cod_data_source_block           2-Me
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0569P)^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^)+(0.0569P)^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_original_cell_volume        1185.7(4)
_cod_original_formula_sum        'C24 H32 Cl2 N2 O0.50 W'
_cod_database_code               4113830
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W -0.36889(3) -0.09935(2) 0.229501(14) 0.01739(9) Uani 1 d .
Cl1 Cl -0.5558(2) 0.01625(13) 0.30097(10) 0.0280(3) Uani 1 d .
Cl2 Cl -0.6104(2) -0.28325(13) 0.19164(11) 0.0294(3) Uani 1 d .
N1 N -0.3162(6) 0.0599(4) 0.1681(3) 0.0189(9) Uani 1 d .
N2 N -0.3649(6) -0.1761(4) 0.0787(3) 0.0197(9) Uani 1 d .
C1 C -0.0871(7) -0.0123(6) 0.3272(4) 0.0285(12) Uani 1 d .
C2 C -0.1917(7) -0.0161(6) 0.3949(4) 0.0286(12) Uani 1 d .
C3 C -0.2796(7) -0.1471(5) 0.3784(4) 0.0247(11) Uani 1 d .
C4 C -0.2219(7) -0.2238(5) 0.3011(4) 0.0247(11) Uani 1 d .
C5 C -0.1046(7) -0.1390(6) 0.2701(4) 0.0274(12) Uani 1 d .
C6 C 0.0356(9) 0.1037(7) 0.3205(7) 0.054(2) Uani 1 d .
H6A H 0.1404(9) 0.1178(7) 0.3688(7) 0.080 Uiso 1 d R
H6B H 0.0535(9) 0.0888(7) 0.2535(7) 0.080 Uiso 1 d R
H6C H -0.0081(9) 0.1786(7) 0.3349(7) 0.080 Uiso 1 d R
C7 C -0.1979(10) 0.0960(7) 0.4766(5) 0.050(2) Uani 1 d .
H7A H -0.1108(10) 0.1078(7) 0.5361(5) 0.080 Uiso 1 d R
H7B H -0.1813(10) 0.1729(7) 0.4536(5) 0.080 Uiso 1 d R
H7C H -0.3056(10) 0.0794(7) 0.4925(5) 0.080 Uiso 1 d R
C8 C -0.3932(10) -0.1990(9) 0.4393(5) 0.054(2) Uani 1 d .
H8A H -0.3271(10) -0.2117(9) 0.4987(5) 0.080 Uiso 1 d R
H8B H -0.4564(10) -0.1378(9) 0.4591(5) 0.080 Uiso 1 d R
H8C H -0.4692(10) -0.2800(9) 0.3992(5) 0.080 Uiso 1 d R
C9 C -0.2579(10) -0.3694(6) 0.2733(6) 0.050(2) Uani 1 d .
H9A H -0.1744(10) -0.3946(6) 0.3167(6) 0.080 Uiso 1 d R
H9B H -0.3673(10) -0.4048(6) 0.2818(6) 0.080 Uiso 1 d R
H9C H -0.2550(10) -0.4014(6) 0.2041(6) 0.080 Uiso 1 d R
C10 C -0.0060(9) -0.1790(9) 0.1946(5) 0.051(2) Uani 1 d .
H10A H 0.0986(9) -0.1900(9) 0.2292(5) 0.080 Uiso 1 d R
H10B H -0.0695(9) -0.2591(9) 0.1461(5) 0.080 Uiso 1 d R
H10C H 0.0162(9) -0.1130(9) 0.1602(5) 0.080 Uiso 1 d R
C11 C -0.2839(8) 0.1848(5) 0.2240(4) 0.0252(12) Uani 1 d .
H11A H -0.3058(8) 0.2011(5) 0.2900(4) 0.080 Uiso 1 d R
C12 C -0.2206(8) 0.2876(5) 0.1904(4) 0.0281(12) Uani 1 d .
H12A H -0.1961(8) 0.3741(5) 0.2334(4) 0.080 Uiso 1 d R
C13 C -0.1913(7) 0.2684(5) 0.0923(4) 0.0260(12) Uani 1 d .
C14 C -0.2301(7) 0.1422(5) 0.0342(4) 0.0253(11) Uani 1 d .
H14A H -0.2161(7) 0.1248(5) -0.0337(4) 0.080 Uiso 1 d R
C15 C -0.2910(7) 0.0398(5) 0.0721(4) 0.0198(10) Uani 1 d .
C16 C -0.1164(9) 0.3804(6) 0.0566(5) 0.038(2) Uani 1 d .
H16A H -0.1053(9) 0.3495(6) -0.0111(5) 0.080 Uiso 1 d R
H16B H -0.1888(9) 0.4381(6) 0.0572(5) 0.080 Uiso 1 d R
H16C H -0.0075(9) 0.4255(6) 0.1005(5) 0.080 Uiso 1 d R
C17 C -0.3844(7) -0.3067(5) 0.0361(4) 0.0244(11) Uani 1 d .
H17A H -0.4127(7) -0.3659(5) 0.0752(4) 0.080 Uiso 1 d R
C18 C -0.3657(8) -0.3543(5) -0.0575(4) 0.0271(12) Uani 1 d .
H18A H -0.3785(8) -0.4457(5) -0.0826(4) 0.080 Uiso 1 d R
C19 C -0.3287(8) -0.2728(5) -0.1198(4) 0.0263(12) Uani 1 d .
C20 C -0.3067(7) -0.1420(5) -0.0777(4) 0.0250(11) Uani 1 d .
H20A H -0.2795(7) -0.0821(5) -0.1165(4) 0.080 Uiso 1 d R
C21 C -0.3221(7) -0.0949(5) 0.0204(4) 0.0199(10) Uani 1 d .
C22 C -0.3144(10) -0.3269(6) -0.2251(5) 0.042(2) Uani 1 d .
H22A H -0.2888(10) -0.2575(6) -0.2557(5) 0.080 Uiso 1 d R
H22B H -0.2258(10) -0.3706(6) -0.2223(5) 0.080 Uiso 1 d R
H22C H -0.4186(10) -0.3869(6) -0.2646(5) 0.080 Uiso 1 d R
O1 O 0.0691(25) 0.5083(20) -0.4647(13) 0.107(3) Uiso 0.50 d PD
C100 C 0.1506(31) 0.5108(32) -0.5459(19) 0.107(3) Uiso 0.50 d PD
H10D H 0.1353(31) 0.5789(32) -0.5769(19) 0.080 Uiso 0.50 d PR
H10E H 0.1081(31) 0.4285(32) -0.5958(19) 0.080 Uiso 0.50 d PR
C101 C 0.3257(28) 0.5444(27) -0.5016(20) 0.107(3) Uiso 0.50 d PD
H10F H 0.3959(28) 0.5441(27) -0.5484(20) 0.080 Uiso 0.50 d PR
H10G H 0.3614(28) 0.6261(27) -0.4509(20) 0.080 Uiso 0.50 d PR
H10H H 0.3343(28) 0.4760(27) -0.4697(20) 0.080 Uiso 0.50 d PR
C200 C -0.0952(34) 0.4613(31) -0.5005(21) 0.107(3) Uiso 0.50 d PD
H20B H -0.1370(34) 0.4082(31) -0.5690(21) 0.080 Uiso 0.50 d PR
H20C H -0.1034(34) 0.5478(31) -0.4992(21) 0.080 Uiso 0.50 d PR
C201 C -0.1773(34) 0.4634(29) -0.4137(20) 0.107(3) Uiso 0.50 d PD
H20D H -0.2932(34) 0.4624(29) -0.4371(20) 0.080 Uiso 0.50 d PR
H20E H -0.1682(34) 0.3770(29) -0.4156(20) 0.080 Uiso 0.50 d PR
H20F H -0.1344(34) 0.5175(29) -0.3454(20) 0.080 Uiso 0.50 d PR
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'
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'
O O 0.0106 0.0060 '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
N2 W1 N1 73.5(2) . .
N2 W1 C4 98.0(2) . .
N1 W1 C4 137.2(2) . .
N2 W1 C3 134.6(2) . .
N1 W1 C3 137.2(2) . .
C4 W1 C3 36.7(2) . .
N2 W1 C5 85.2(2) . .
N1 W1 C5 101.6(2) . .
C4 W1 C5 35.6(2) . .
C3 W1 C5 59.9(2) . .
N2 W1 C2 141.9(2) . .
N1 W1 C2 101.7(2) . .
C4 W1 C2 59.3(2) . .
C3 W1 C2 35.5(2) . .
C5 W1 C2 58.3(2) . .
N2 W1 C1 108.3(2) . .
N1 W1 C1 83.8(2) . .
C4 W1 C1 58.6(2) . .
C3 W1 C1 58.9(2) . .
C5 W1 C1 34.7(2) . .
C2 W1 C1 34.6(2) . .
N2 W1 Cl1 131.21(13) . .
N1 W1 Cl1 83.17(12) . .
C4 W1 Cl1 126.8(2) . .
C3 W1 Cl1 91.01(15) . .
C5 W1 Cl1 142.18(14) . .
C2 W1 Cl1 83.92(14) . .
C1 W1 Cl1 111.0(2) . .
N2 W1 Cl2 83.70(12) . .
N1 W1 Cl2 133.37(13) . .
C4 W1 Cl2 85.1(2) . .
C3 W1 Cl2 87.1(2) . .
C5 W1 Cl2 116.6(2) . .
C2 W1 Cl2 120.4(2) . .
C1 W1 Cl2 142.62(15) . .
Cl1 W1 Cl2 82.32(5) . .
C11 N1 C15 117.2(4) . .
C11 N1 W1 122.7(3) . .
C15 N1 W1 119.5(3) . .
C21 N2 C17 116.2(4) . .
C21 N2 W1 120.2(3) . .
C17 N2 W1 123.2(3) . .
C5 C1 C2 108.8(5) . .
C5 C1 C6 123.7(6) . .
C2 C1 C6 127.3(6) . .
C5 C1 W1 71.0(3) . .
C2 C1 W1 72.4(3) . .
C6 C1 W1 126.5(4) . .
C1 C2 C3 108.1(5) . .
C1 C2 C7 126.2(6) . .
C3 C2 C7 125.5(6) . .
C1 C2 W1 73.0(3) . .
C3 C2 W1 69.1(3) . .
C7 C2 W1 127.7(4) . .
C2 C3 C4 107.0(5) . .
C2 C3 C8 126.9(6) . .
C4 C3 C8 125.7(6) . .
C2 C3 W1 75.3(3) . .
C4 C3 W1 71.4(3) . .
C8 C3 W1 124.9(4) . .
C5 C4 C3 107.9(5) . .
C5 C4 C9 126.5(6) . .
C3 C4 C9 124.8(6) . .
C5 C4 W1 74.2(3) . .
C3 C4 W1 71.9(3) . .
C9 C4 W1 128.0(4) . .
C1 C5 C4 108.2(5) . .
C1 C5 C10 126.0(6) . .
C4 C5 C10 125.7(6) . .
C1 C5 W1 74.3(3) . .
C4 C5 W1 70.2(3) . .
C10 C5 W1 124.7(4) . .
N1 C11 C12 122.7(5) . .
C11 C12 C13 120.7(5) . .
C14 C13 C12 116.7(5) . .
C14 C13 C16 122.5(5) . .
C12 C13 C16 120.8(5) . .
C13 C14 C15 120.9(5) . .
N1 C15 C14 121.8(4) . .
N1 C15 C21 113.2(4) . .
C14 C15 C21 124.9(5) . .
C18 C17 N2 123.1(5) . .
C17 C18 C19 121.3(5) . .
C20 C19 C18 116.1(5) . .
C20 C19 C22 122.9(5) . .
C18 C19 C22 121.0(5) . .
C19 C20 C21 121.4(5) . .
N2 C21 C20 121.8(4) . .
N2 C21 C15 113.3(4) . .
C20 C21 C15 124.9(5) . .
C200 O1 O1 74.8(35) 2_564 2_564
C200 O1 C200 105.2(37) 2_564 .
O1 O1 C200 30.4(14) 2_564 .
C200 O1 C100 29.8(34) 2_564 .
O1 O1 C100 84.1(19) 2_564 .
C200 O1 C100 110.6(17) . .
C200 O1 C100 119.1(42) 2_564 2_564
O1 O1 C100 50.5(15) 2_564 2_564
C200 O1 C100 27.1(14) . 2_564
C100 O1 C100 134.7(13) . 2_564
C201 C100 C200 132.8(60) 2_564 2_564
C201 C100 C101 83.4(35) 2_564 .
C200 C100 C101 110.3(36) 2_564 .
C201 C100 O1 155.1(49) 2_564 .
C200 C100 O1 22.4(26) 2_564 .
C101 C100 O1 106.4(19) . .
C201 C100 O1 120.0(41) 2_564 2_564
C200 C100 O1 41.9(24) 2_564 2_564
C101 C100 O1 151.2(21) . 2_564
O1 C100 O1 45.3(13) . 2_564
C100 C101 C201 28.8(13) . 2_564
C100 C101 C200 26.1(14) . 2_564
C201 C101 C200 50.1(14) 2_564 2_564
O1 C200 C100 127.8(57) 2_564 2_564
O1 C200 O1 74.8(37) 2_564 .
C100 C200 O1 111.0(35) 2_564 .
O1 C200 C201 148.8(47) 2_564 .
C100 C200 C201 21.1(28) 2_564 .
O1 C200 C201 109.3(21) . .
O1 C200 C200 50.9(27) 2_564 2_564
C100 C200 C200 123.1(44) 2_564 2_564
O1 C200 C200 24.0(14) . 2_564
C201 C200 C200 128.7(30) . 2_564
O1 C200 C101 112.7(43) 2_564 2_564
C100 C200 C101 43.6(26) 2_564 2_564
O1 C200 C101 153.5(21) . 2_564
C201 C200 C101 50.8(14) . 2_564
C200 C200 C101 151.8(33) 2_564 2_564
C100 C201 C200 26.1(34) 2_564 .
C100 C201 C101 67.8(33) 2_564 2_564
C200 C201 C101 79.1(19) . 2_564
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 N2 2.098(4) .
W1 N1 2.115(4) .
W1 C4 2.276(5) .
W1 C3 2.283(5) .
W1 C5 2.328(5) .
W1 C2 2.363(5) .
W1 C1 2.371(5) .
W1 Cl1 2.4246(15) .
W1 Cl2 2.429(2) .
N1 C11 1.361(6) .
N1 C15 1.374(7) .
N2 C21 1.373(6) .
N2 C17 1.385(6) .
C1 C5 1.402(8) .
C1 C2 1.408(9) .
C1 C6 1.497(8) .
C2 C3 1.420(8) .
C2 C7 1.497(8) .
C3 C4 1.437(8) .
C3 C8 1.503(9) .
C4 C5 1.410(8) .
C4 C9 1.507(8) .
C5 C10 1.503(8) .
C11 C12 1.364(8) .
C12 C13 1.416(8) .
C13 C14 1.376(7) .
C13 C16 1.494(8) .
C14 C15 1.391(7) .
C15 C21 1.437(7) .
C17 C18 1.348(8) .
C18 C19 1.410(8) .
C19 C20 1.382(8) .
C19 C22 1.496(7) .
C20 C21 1.394(7) .
O1 C200 0.69(3) 2_564
O1 O1 1.32(4) 2_564
O1 C200 1.32(2) .
O1 C100 1.43(2) .
O1 C100 1.85(4) 2_564
C100 C201 0.74(3) 2_564
C100 C200 0.90(3) 2_564
C100 C101 1.41(2) .
C100 O1 1.85(4) 2_564
C101 C201 1.52(4) 2_564
C101 C200 1.92(4) 2_564
C200 O1 0.69(3) 2_564
C200 C100 0.90(3) 2_564
C200 C201 1.50(2) .
C200 C200 1.64(5) 2_564
C200 C101 1.92(4) 2_564
C201 C100 0.74(3) 2_564
C201 C101 1.52(4) 2_564
