#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:14:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179318 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/15/4321562.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_4321562
loop_
_publ_author_name
'F. Albert Cotton'
'Evgeny V. Dikarev'
'Jiande Gu'
'Santiago Herrero'
'Barbara Modec'
_publ_section_title
;
 Alkylpyridine Complexes of Tungsten(II) and Chromium(II). First
 Rotational Isomers of W2X4L4 Molecules with D2 hand D2 Symmetries
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5407
_journal_page_last               5411
_journal_paper_doi               10.1021/ic000555v
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'W2 Cl4 (N C5 H4 C (C H3)3)4, C7 H8'
_chemical_formula_structural     '(D2h)-W2Cl4(4-t-Bu-py)4, C7H8'
_chemical_formula_sum            'C43 H60 Cl4 N4 W2'
_chemical_formula_weight         1142.45
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Bis(trans-dichloro-bis(4-tert-butylpyridine))-di-tungsten (II),
 D2h isomer, toluene solvate
;
_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
_cell_angle_alpha                107.88(3)
_cell_angle_beta                 105.68(1)
_cell_angle_gamma                99.16(2)
_cell_formula_units_Z            1
_cell_length_a                   8.556(1)
_cell_length_b                   11.809(2)
_cell_length_c                   12.696(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.0
_cell_volume                     1133.6(5)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6159
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.56
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    5.339
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.565
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.045
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.058
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_obs          0.0372
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0082P)²+16.0157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0891
_refine_ls_wR_factor_obs         0.0845
_reflns_number_observed          2669
_reflns_number_total             2875
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000555v_3.cif
_cod_data_source_block           W2Cl4(4-t-Bu-py)4,C7H8_(1a,C7H8)
_cod_depositor_comments
;
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 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0082P)^2^+16.0157P] 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^)+(0.0082P)^2^+16.0157P] 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        1133.6(4)
_cod_database_code               4321562
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
_atom_site_disorder_group
W1 W -0.03057(4) 0.08331(3) -0.01808(3) 0.02057(14) Uani 1 d . .
N1 N 0.2017(9) 0.2282(6) 0.0994(6) 0.024(2) Uani 1 d . .
N2 N -0.2771(9) -0.0031(6) -0.1602(6) 0.026(2) Uani 1 d . .
Cl1 Cl 0.0705(3) 0.1004(2) -0.1738(2) 0.0294(5) Uani 1 d . .
Cl2 Cl -0.1678(3) 0.1568(2) 0.1205(2) 0.0284(5) Uani 1 d . .
C1 C 0.3511(11) 0.2200(8) 0.0871(8) 0.027(2) Uani 1 d . .
H1A H 0.3541(11) 0.1491(8) 0.0290(8) 0.032 Uiso 1 calc R .
C2 C 0.4983(12) 0.3083(8) 0.1538(9) 0.033(2) Uani 1 d . .
H2A H 0.5989(12) 0.2960(8) 0.1416(9) 0.040 Uiso 1 calc R .
C3 C 0.5019(13) 0.4161(9) 0.2395(9) 0.038(3) Uani 1 d . .
C4 C 0.3466(12) 0.4259(8) 0.2500(8) 0.035(2) Uani 1 d U .
H4A H 0.3403(12) 0.4968(8) 0.3063(8) 0.042 Uiso 1 calc R .
C5 C 0.2019(12) 0.3336(8) 0.1795(9) 0.032(2) Uani 1 d . .
H5A H 0.0989(12) 0.3448(8) 0.1877(9) 0.038 Uiso 1 calc R .
C6 C 0.6640(13) 0.5168(9) 0.3206(10) 0.048(3) Uani 1 d D 1
C7 C 0.8227(25) 0.4754(22) 0.3163(24) 0.020(7) Uiso 0.40 d PD 1
H7A H 0.9210(25) 0.5425(22) 0.3691(24) 0.030 Uiso 0.40 calc PR 1
H7B H 0.8252(25) 0.4524(22) 0.2367(24) 0.030 Uiso 0.40 calc PR 1
H7C H 0.8230(25) 0.4050(22) 0.3404(24) 0.030 Uiso 0.40 calc PR 1
C8 C 0.6629(39) 0.6275(24) 0.2807(30) 0.048(9) Uiso 0.40 d PD 1
H8A H 0.5620(39) 0.6541(24) 0.2834(30) 0.072 Uiso 0.40 calc PR 1
H8B H 0.6648(39) 0.6034(24) 0.2010(30) 0.072 Uiso 0.40 calc PR 1
H8C H 0.7613(39) 0.6948(24) 0.3328(30) 0.072 Uiso 0.40 calc PR 1
C9 C 0.6673(57) 0.5695(42) 0.4496(25) 0.103(18) Uiso 0.40 d PD 1
H9A H 0.5655(57) 0.5954(42) 0.4507(25) 0.155 Uiso 0.40 calc PR 1
H9B H 0.7646(57) 0.6398(42) 0.4952(25) 0.155 Uiso 0.40 calc PR 1
H9C H 0.6740(57) 0.5064(42) 0.4834(25) 0.155 Uiso 0.40 calc PR 1
C7X C 0.7766(88) 0.4653(65) 0.3968(53) 0.114(31) Uiso 0.200(6) d PD 2
H7XA H 0.7226(88) 0.4439(65) 0.4487(53) 0.170 Uiso 0.20 calc PR 2
H7XB H 0.8830(88) 0.5268(65) 0.4434(53) 0.170 Uiso 0.20 calc PR 2
H7XC H 0.7965(88) 0.3922(65) 0.3473(53) 0.170 Uiso 0.20 calc PR 2
C8X C 0.7432(55) 0.5517(40) 0.2378(33) 0.028(11) Uiso 0.20 d PD 2
H8XA H 0.6682(55) 0.5845(40) 0.1901(33) 0.042 Uiso 0.20 calc PR 2
H8XB H 0.7628(55) 0.4792(40) 0.1870(33) 0.042 Uiso 0.20 calc PR 2
H8XC H 0.8495(55) 0.6138(40) 0.2832(33) 0.042 Uiso 0.20 calc PR 2
C9X C 0.6270(74) 0.6347(39) 0.3919(48) 0.059(17) Uiso 0.20 d PD 2
H9XA H 0.5544(74) 0.6634(39) 0.3385(48) 0.089 Uiso 0.20 calc PR 2
H9XB H 0.7319(74) 0.6982(39) 0.4377(48) 0.089 Uiso 0.20 calc PR 2
H9XC H 0.5715(74) 0.6166(39) 0.4444(48) 0.089 Uiso 0.20 calc PR 2
C7Y C 0.8172(30) 0.4918(26) 0.2866(27) 0.035(9) Uiso 0.400(6) d PD 3
H7YA H 0.8304(30) 0.4124(26) 0.2888(27) 0.053 Uiso 0.40 calc PR 3
H7YB H 0.9173(30) 0.5560(26) 0.3417(27) 0.053 Uiso 0.40 calc PR 3
H7YC H 0.8011(30) 0.4912(26) 0.2078(27) 0.053 Uiso 0.40 calc PR 3
C8Y C 0.6403(37) 0.6395(21) 0.3180(27) 0.041(8) Uiso 0.40 d PD 3
H8YA H 0.5427(37) 0.6536(21) 0.3398(27) 0.061 Uiso 0.40 calc PR 3
H8YB H 0.6233(37) 0.6396(21) 0.2394(27) 0.061 Uiso 0.40 calc PR 3
H8YC H 0.7395(37) 0.7044(21) 0.3732(27) 0.061 Uiso 0.40 calc PR 3
C9Y C 0.6939(31) 0.5286(25) 0.4526(16) 0.025(6) Uiso 0.40 d PD 3
H9YA H 0.7104(31) 0.4520(25) 0.4610(16) 0.038 Uiso 0.40 calc PR 3
H9YB H 0.5967(31) 0.5456(25) 0.4734(16) 0.038 Uiso 0.40 calc PR 3
H9YC H 0.7930(31) 0.5955(25) 0.5043(16) 0.038 Uiso 0.40 calc PR 3
C10 C -0.2911(11) -0.0871(8) -0.2632(7) 0.027(2) Uani 1 d . .
H10A H -0.1973(11) -0.1163(8) -0.2711(7) 0.033 Uiso 1 calc R .
C11 C -0.4384(12) -0.1321(8) -0.3579(8) 0.028(2) Uani 1 d . .
H11A H -0.4443(12) -0.1943(8) -0.4272(8) 0.034 Uiso 1 calc R .
C12 C -0.5789(11) -0.0879(8) -0.3537(8) 0.025(2) Uani 1 d . .
C13 C -0.5623(11) -0.0036(8) -0.2455(8) 0.027(2) Uani 1 d . .
H13A H -0.6546(11) 0.0265(8) -0.2352(8) 0.032 Uiso 1 calc R .
C14 C -0.4145(11) 0.0369(8) -0.1531(7) 0.026(2) Uani 1 d . .
H14A H -0.4081(11) 0.0953(8) -0.0814(7) 0.031 Uiso 1 calc R .
C15 C -0.7388(11) -0.1251(9) -0.4580(8) 0.033(2) Uani 1 d U .
C16 C -0.7281(15) -0.2109(13) -0.5703(10) 0.068(4) Uani 1 d U .
H16A H -0.8336(15) -0.2316(13) -0.6339(10) 0.103 Uiso 1 calc R .
H16B H -0.7064(15) -0.2856(13) -0.5600(10) 0.103 Uiso 1 calc R .
H16C H -0.6374(15) -0.1705(13) -0.5893(10) 0.103 Uiso 1 calc R .
C17 C -0.8874(12) -0.1828(10) -0.4295(9) 0.045(3) Uani 1 d U .
H17A H -0.8920(12) -0.1263(10) -0.3572(9) 0.067 Uiso 1 calc R .
H17B H -0.8735(12) -0.2594(10) -0.4200(9) 0.067 Uiso 1 calc R .
H17C H -0.9912(12) -0.1994(10) -0.4933(9) 0.067 Uiso 1 calc R .
C18 C -0.7705(16) -0.0070(13) -0.4767(11) 0.068(4) Uani 1 d . .
H18A H -0.7778(16) 0.0494(13) -0.4054(11) 0.103 Uiso 1 calc R .
H18B H -0.8752(16) -0.0278(13) -0.5410(11) 0.103 Uiso 1 calc R .
H18C H -0.6785(16) 0.0319(13) -0.4955(11) 0.103 Uiso 1 calc R .
C19 C 0.0316(49) 0.5291(32) 0.0226(32) 0.080(10) Uiso 0.50 d P .
C20 C -0.1316(37) 0.5644(25) 0.0447(24) 0.065(7) Uiso 0.50 d P .
C21 C -0.2786(45) 0.4777(33) -0.0100(31) 0.091(10) Uiso 0.50 d P .
C22 C -0.3069(44) 0.3663(30) -0.0777(28) 0.076(8) Uiso 0.50 d P .
C23 C -0.1599(31) 0.3402(23) -0.1001(22) 0.049(6) Uiso 0.50 d P .
C24 C -0.0021(31) 0.4102(22) -0.0634(21) 0.045(6) Uiso 0.50 d P .
C25 C 0.1928(71) 0.6067(50) 0.0626(46) 0.131(17) Uiso 0.50 d P .
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 N2 157.7(3) . . y
N1 W1 W1 101.1(2) . 2 y
N2 W1 W1 100.7(2) . 2 y
N1 W1 Cl2 89.7(2) . . y
N2 W1 Cl2 90.2(2) . . y
W1 W1 Cl2 101.92(6) 2 . y
N1 W1 Cl1 84.9(2) . . y
N2 W1 Cl1 84.3(2) . . y
W1 W1 Cl1 107.61(6) 2 . y
Cl2 W1 Cl1 150.47(8) . . y
C5 N1 C1 116.0(7) . . n
C5 N1 W1 122.8(6) . . n
C1 N1 W1 120.9(6) . . n
C10 N2 C14 116.9(8) . . n
C10 N2 W1 120.7(6) . . n
C14 N2 W1 121.8(6) . . n
N1 C1 C2 123.9(8) . . n
C1 C2 C3 120.9(9) . . n
C2 C3 C4 115.1(9) . . n
C2 C3 C6 123.5(9) . . n
C4 C3 C6 121.3(9) . . n
C5 C4 C3 121.2(8) . . n
N1 C5 C4 122.7(9) . . n
C7 C6 C3 113.0(12) . . n
C7 C6 C8 109.3(17) . . n
C3 C6 C8 107.2(15) . . n
C7 C6 C9 110.6(19) . . n
C3 C6 C9 112.4(19) . . n
C8 C6 C9 103.8(19) . . n
C7X C6 C8X 111.4(25) . . n
C7X C6 C3 109.5(32) . . n
C8X C6 C3 104.6(19) . . n
C7X C6 C9X 113.2(25) . . n
C8X C6 C9X 105.9(21) . . n
C3 C6 C9X 111.9(24) . . n
C8Y C6 C7Y 110.7(17) . . n
C8Y C6 C3 109.0(14) . . n
C7Y C6 C3 112.2(13) . . n
C8Y C6 C9Y 104.8(15) . . n
C7Y C6 C9Y 110.3(16) . . n
C3 C6 C9Y 109.6(12) . . n
N2 C10 C11 122.1(8) . . n
C10 C11 C12 121.6(8) . . n
C13 C12 C11 114.9(8) . . n
C13 C12 C15 121.0(8) . . n
C11 C12 C15 124.1(8) . . n
C14 C13 C12 121.3(8) . . n
N2 C14 C13 123.0(8) . . n
C16 C15 C12 113.1(8) . . n
C16 C15 C17 110.9(9) . . n
C12 C15 C17 109.6(8) . . n
C16 C15 C18 108.2(10) . . n
C12 C15 C18 107.7(8) . . n
C17 C15 C18 107.3(9) . . n
C25 C19 C24 117.7(43) . . n
C25 C19 C20 127.5(38) . . n
C24 C19 C20 113.9(24) . . n
C21 C20 C19 118.0(27) . . n
C22 C21 C20 128.4(36) . . n
C21 C22 C23 111.9(32) . . n
C24 C23 C22 132.0(27) . . n
C23 C24 C19 115.2(31) . . 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 2.202(7) . y
W1 N2 2.207(7) . y
W1 W1 2.2602(8) 2 y
W1 Cl2 2.394(2) . y
W1 Cl1 2.410(2) . y
N1 C5 1.343(11) . n
N1 C1 1.344(11) . n
N2 C10 1.337(11) . n
N2 C14 1.350(11) . n
C1 C2 1.362(13) . n
C2 C3 1.387(13) . n
C3 C4 1.390(14) . n
C3 C6 1.533(14) . n
C4 C5 1.376(13) . n
C6 C7 1.52(2) . n
C6 C8 1.54(2) . n
C6 C9 1.55(2) . n
C6 C7X 1.51(3) . n
C6 C8X 1.52(3) . n
C6 C9X 1.54(3) . n
C6 C8Y 1.50(2) . n
C6 C7Y 1.53(2) . n
C6 C9Y 1.58(2) . n
C10 C11 1.376(13) . n
C11 C12 1.393(13) . n
C12 C13 1.381(13) . n
C12 C15 1.513(13) . n
C13 C14 1.365(12) . n
C15 C16 1.511(14) . n
C15 C17 1.528(14) . n
C15 C18 1.54(2) . n
C19 C25 1.39(6) . n
C19 C24 1.42(5) . n
C19 C20 1.59(5) . n
C20 C21 1.34(4) . n
C21 C22 1.27(4) . n
C22 C23 1.42(4) . n
C23 C24 1.34(3) . n
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 W1 W1 N2 4.6(3) . . 2 2 y
Cl1 W1 W1 Cl2 0.14(8) . . 2 2 y
N2 W1 W1 N1 -4.6(3) . . 2 2 y
Cl2 W1 W1 Cl1 -0.14(8) . . 2 2 y
