#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:21:57 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301837 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/18/4311890.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_4311890
loop_
_publ_author_name
'F. Albert Cotton'
'James P. Donahue'
'Michael B. Hall'
'Carlos A. Murillo'
'Dino Villagrán'
_publ_contact_author_phone       979-845-4432
_publ_section_title
;
 Reaction Products of W(CO)6 with Formamidines; Electronic Structure of a
 W2(μ-CO)2 Core with Unsymmetric Bridging Carbonyls
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6954
_journal_page_last               6964
_journal_paper_doi               10.1021/ic049116c
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'W2 ((Cl2 C6 H3 N)2 C H)4'
_chemical_formula_sum            'C52 H28 Cl16 N8 W2'
_chemical_formula_weight         1699.72
_chemical_melting_point          ?
_chemical_name_common            W2(D(Cl)PhF)4
_chemical_name_systematic
;
 Ditungsten(II) tetra(N,N'-3,5-dichlorophenyl)formamidinate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           SHELXL-97
_cell_angle_alpha                97.897(2)
_cell_angle_beta                 104.285(2)
_cell_angle_gamma                113.530(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8234(11)
_cell_length_b                   11.7146(13)
_cell_length_c                   14.3771(16)
_cell_measurement_reflns_used    3828
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.14
_cell_volume                     1417.2(3)
_computing_cell_refinement       'SAINT V. 6.22'
_computing_data_collection       'SMART V. 5.618'
_computing_data_reduction        'SAINT V. 6.22'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9937
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    4.856
_exptl_absorpt_correction_T_max  0.8680
_exptl_absorpt_correction_T_min  0.3413
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.012
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0393P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                5050
_reflns_number_total             6228
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic049116csi20040706_041210_6.cif
_cod_data_source_block           W2(D(Cl)PhF)4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (15
times).

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (32
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (24
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (48 times).

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:
data name '_publ_contact_author-phone' replaced with
'_publ_contact_author_phone' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_database_code               4311890
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_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 -1.43841(2) -0.01294(2) 0.569316(18) 0.01809(8) Uani 1 1 d . . .
Cl1 Cl -1.18991(18) -0.47526(16) 0.48424(14) 0.0384(4) Uani 1 1 d . . .
Cl2 Cl -1.3186(2) -0.33699(17) 0.81111(13) 0.0415(4) Uani 1 1 d . . .
Cl3 Cl -1.93286(18) -0.46676(16) 0.74542(14) 0.0377(4) Uani 1 1 d . . .
Cl4 Cl -1.3771(2) -0.0648(2) 0.96509(14) 0.0523(5) Uani 1 1 d . . .
Cl5 Cl -0.9856(2) 0.17801(19) 0.96016(13) 0.0443(4) Uani 1 1 d . . .
Cl6 Cl -1.2857(2) 0.47180(17) 0.98530(13) 0.0419(4) Uani 1 1 d . . .
Cl7 Cl -0.66319(17) 0.39719(16) 0.76550(14) 0.0384(4) Uani 1 1 d . . .
Cl8 Cl -0.92315(19) -0.08619(16) 0.80277(14) 0.0405(4) Uani 1 1 d . . .
N1 N -1.4917(5) -0.2036(4) 0.4959(4) 0.0205(10) Uani 1 1 d . . .
N2 N -1.6493(5) -0.0878(4) 0.6067(4) 0.0220(11) Uani 1 1 d . . .
N3 N -1.3751(5) 0.1790(4) 0.6506(4) 0.0212(10) Uani 1 1 d . . .
N4 N -1.2221(5) 0.0598(4) 0.5394(3) 0.0192(10) Uani 1 1 d . . .
C1 C -1.5748(6) -0.2501(5) 0.3995(4) 0.0236(13) Uani 1 1 d . . .
H1 H -1.5984 -0.3340 0.3663 0.028 Uiso 1 1 calc R . .
C2 C -1.4224(6) -0.2770(5) 0.5417(5) 0.0229(13) Uani 1 1 d . . .
C3 C -1.3531(6) -0.3385(6) 0.4930(5) 0.0257(13) Uani 1 1 d . . .
H3 H -1.3582 -0.3386 0.4269 0.031 Uiso 1 1 calc R . .
C4 C -1.2771(6) -0.3990(5) 0.5448(5) 0.0258(13) Uani 1 1 d . . .
C5 C -1.2621(6) -0.3976(5) 0.6433(5) 0.0276(14) Uani 1 1 d . . .
H5 H -1.2046 -0.4352 0.6781 0.033 Uiso 1 1 calc R . .
C6 C -1.3345(6) -0.3392(6) 0.6879(5) 0.0251(13) Uani 1 1 d . . .
C7 C -1.4153(6) -0.2799(5) 0.6396(5) 0.0238(13) Uani 1 1 d . . .
H7 H -1.4651 -0.2419 0.6720 0.029 Uiso 1 1 calc R . .
C8 C -1.7819(6) -0.1003(6) 0.5425(5) 0.0241(13) Uani 1 1 d . . .
H8 H -1.8775 -0.1375 0.5551 0.029 Uiso 1 1 calc R . .
C9 C -1.6622(6) -0.1444(6) 0.6871(5) 0.0227(13) Uani 1 1 d . . .
C10 C -1.7835(6) -0.2650(5) 0.6770(5) 0.0232(13) Uani 1 1 d . . .
H10 H -1.8662 -0.3101 0.6162 0.028 Uiso 1 1 calc R . .
C11 C -1.7804(6) -0.3173(6) 0.7575(5) 0.0262(13) Uani 1 1 d . . .
C12 C -1.6564(7) -0.2592(6) 0.8461(5) 0.0324(15) Uani 1 1 d . . .
H12 H -1.6536 -0.2991 0.8985 0.039 Uiso 1 1 calc R . .
C13 C -1.5366(7) -0.1402(7) 0.8551(5) 0.0337(15) Uani 1 1 d . . .
C14 C -1.5373(7) -0.0805(6) 0.7786(5) 0.0295(14) Uani 1 1 d . . .
H14 H -1.4558 0.0016 0.7873 0.035 Uiso 1 1 calc R . .
C15 C -1.2940(6) 0.2338(5) 0.7552(4) 0.0215(12) Uani 1 1 d . . .
C16 C -1.1867(7) 0.1912(6) 0.8017(5) 0.0265(13) Uani 1 1 d . . .
H16 H -1.1653 0.1324 0.7638 0.032 Uiso 1 1 calc R . .
C17 C -1.1126(7) 0.2367(6) 0.9039(5) 0.0280(14) Uani 1 1 d . . .
C18 C -1.1393(7) 0.3229(6) 0.9628(5) 0.0293(14) Uani 1 1 d . . .
H18 H -1.0880 0.3528 1.0320 0.035 Uiso 1 1 calc R . .
C19 C -1.2456(7) 0.3638(5) 0.9151(5) 0.0264(13) Uani 1 1 d . . .
C20 C -1.3250(7) 0.3189(6) 0.8135(5) 0.0256(13) Uani 1 1 d . . .
H20 H -1.3996 0.3459 0.7842 0.031 Uiso 1 1 calc R . .
C21 C -1.0737(6) 0.0892(6) 0.6107(5) 0.0234(13) Uani 1 1 d . . .
C22 C -0.9500(6) 0.2128(6) 0.6433(5) 0.0254(13) Uani 1 1 d . . .
H22 H -0.9561 0.2769 0.6120 0.031 Uiso 1 1 calc R . .
C23 C -0.8165(6) 0.2414(6) 0.7227(5) 0.0286(14) Uani 1 1 d . . .
C24 C -0.8041(7) 0.1501(6) 0.7722(5) 0.0307(15) Uani 1 1 d . . .
H24 H -0.7141 0.1712 0.8265 0.037 Uiso 1 1 calc R . .
C25 C -0.9275(7) 0.0282(6) 0.7390(5) 0.0259(13) Uani 1 1 d . . .
C26 C -1.0623(6) -0.0037(6) 0.6600(4) 0.0240(13) Uani 1 1 d . . .
H26 H -1.1459 -0.0876 0.6395 0.029 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'
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'
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
N1 W1 N4 89.99(17) . . y
N1 W1 N2 89.83(17) . . y
N4 W1 N2 176.85(18) . . y
N1 W1 N3 176.70(18) . . y
N4 W1 N3 89.21(17) . . y
N2 W1 N3 90.79(17) . . y
N1 W1 W1 91.19(13) . 2_256 y
N4 W1 W1 91.64(12) . 2_256 y
N2 W1 W1 91.50(13) . 2_256 y
N3 W1 W1 92.04(12) . 2_256 y
C1 N1 C2 117.7(5) . . y
C1 N1 W1 119.0(4) . . y
C2 N1 W1 122.6(4) . . y
C8 N2 C9 117.5(5) . . y
C8 N2 W1 118.3(4) . . y
C9 N2 W1 123.4(4) . . y
C1 N3 C15 117.0(5) 2_256 . y
C1 N3 W1 117.1(4) 2_256 . y
C15 N3 W1 125.8(4) . . y
C8 N4 C21 116.9(5) 2_256 . y
C8 N4 W1 118.8(4) 2_256 . y
C21 N4 W1 123.3(4) . . y
N1 C1 N3 120.7(5) . 2_256 y
C7 C2 C3 119.8(5) . . n
C7 C2 N1 118.7(5) . . n
C3 C2 N1 121.4(5) . . n
C4 C3 C2 118.2(6) . . n
C5 C4 C3 122.9(6) . . n
C5 C4 Cl1 118.8(5) . . n
C3 C4 Cl1 118.2(5) . . n
C6 C5 C4 117.3(5) . . n
C5 C6 C7 122.6(6) . . n
C5 C6 Cl2 118.3(5) . . n
C7 C6 Cl2 119.1(5) . . n
C6 C7 C2 119.1(6) . . n
N4 C8 N2 119.7(5) 2_256 . y
C10 C9 C14 119.2(5) . . n
C10 C9 N2 123.1(5) . . n
C14 C9 N2 117.5(5) . . n
C11 C10 C9 119.2(6) . . n
C12 C11 C10 122.6(6) . . n
C12 C11 Cl3 118.1(5) . . n
C10 C11 Cl3 119.2(5) . . n
C11 C12 C13 117.6(6) . . n
C14 C13 C12 122.2(6) . . n
C14 C13 Cl4 118.8(5) . . n
C12 C13 Cl4 119.0(5) . . n
C13 C14 C9 119.1(6) . . n
C20 C15 C16 118.8(6) . . n
C20 C15 N3 123.2(5) . . n
C16 C15 N3 117.8(5) . . n
C17 C16 C15 119.4(6) . . n
C18 C17 C16 122.7(6) . . n
C18 C17 Cl5 118.9(5) . . n
C16 C17 Cl5 118.4(5) . . n
C17 C18 C19 116.9(6) . . n
C20 C19 C18 122.5(6) . . n
C20 C19 Cl6 118.3(5) . . n
C18 C19 Cl6 119.2(5) . . n
C19 C20 C15 119.7(6) . . n
C22 C21 C26 119.0(5) . . n
C22 C21 N4 121.5(5) . . n
C26 C21 N4 118.8(5) . . n
C21 C22 C23 119.4(5) . . n
C24 C23 C22 122.1(5) . . n
C24 C23 Cl7 118.3(5) . . n
C22 C23 Cl7 119.5(5) . . n
C25 C24 C23 117.7(6) . . n
C24 C25 C26 121.8(6) . . n
C24 C25 Cl8 119.5(5) . . n
C26 C25 Cl8 118.5(5) . . n
C25 C26 C21 120.0(5) . . n
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 N1 2.127(5) . y
W1 N4 2.129(4) . y
W1 N2 2.139(4) . y
W1 N3 2.148(5) . y
W1 W1 2.1904(5) 2_256 y
Cl1 C4 1.748(6) . n
Cl2 C6 1.735(6) . n
Cl3 C11 1.742(6) . n
Cl4 C13 1.739(7) . n
Cl5 C17 1.738(6) . n
Cl6 C19 1.738(6) . n
Cl7 C23 1.737(6) . n
Cl8 C25 1.733(6) . n
N1 C1 1.328(7) . y
N1 C2 1.427(7) . y
N2 C8 1.336(7) . y
N2 C9 1.418(7) . y
N3 C1 1.330(7) 2_256 y
N3 C15 1.429(7) . y
N4 C8 1.333(7) 2_256 y
N4 C21 1.435(7) . y
C1 N3 1.331(7) 2_256 y
C2 C7 1.399(8) . n
C2 C3 1.400(8) . n
C3 C4 1.382(8) . n
C4 C5 1.383(9) . n
C5 C6 1.370(8) . n
C6 C7 1.377(7) . n
C8 N4 1.333(7) 2_256 y
C9 C10 1.397(8) . n
C9 C14 1.412(8) . n
C10 C11 1.380(8) . n
C11 C12 1.380(9) . n
C12 C13 1.382(9) . n
C13 C14 1.382(9) . n
C15 C20 1.388(8) . n
C15 C16 1.404(8) . n
C16 C17 1.386(8) . n
C17 C18 1.375(9) . n
C18 C19 1.387(8) . n
C19 C20 1.385(8) . n
C21 C22 1.386(8) . n
C21 C26 1.402(8) . n
C22 C23 1.393(8) . n
C23 C24 1.391(8) . n
C24 C25 1.371(8) . n
C25 C26 1.389(8) . n
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139130572
