#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:46:10 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179305 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/02/4320289.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_4320289
loop_
_publ_author_name
'R. C. Mills'
'S. Y. S. Wang'
'K. A. Abboud'
'J. M. Boncella'
_publ_section_title
;
 Coordinatively Unsaturated W(IV)-Bis(pyridine) Complexes, a Reactive
 Source of W(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5077
_journal_page_last               5082
_journal_paper_doi               10.1021/ic010195r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H41 N5 Si2 W'
_chemical_formula_weight         711.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 101.720(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6142(7)
_cell_length_b                   12.7895(6)
_cell_length_c                   19.054(1)
_cell_measurement_temperature    173(2)
_cell_volume                     3248.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22571
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    3.656
_exptl_absorpt_correction_T_max  0.8168
_exptl_absorpt_correction_T_min  0.4250
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         7453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0248
_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)+(0.0242P)²+1.8314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                6092
_reflns_number_total             7453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010195r_1.cif
_cod_data_source_block           C30H41N5Si2W
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3248.4(3)
_cod_database_code               4320289
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.302978(9) 0.766774(10) 0.187655(6) 0.03410(5) Uani 1 1 d . . .
Si1 Si 0.07913(7) 0.65541(9) 0.12035(5) 0.0480(2) Uani 1 1 d . . .
Si2 Si 0.48761(6) 0.80951(7) 0.09588(5) 0.03484(18) Uani 1 1 d . . .
N1 N 0.2520(2) 0.8920(2) 0.19185(15) 0.0424(6) Uani 1 1 d . . .
N2 N 0.2067(2) 0.6705(2) 0.11892(13) 0.0391(6) Uani 1 1 d . . .
N3 N 0.38596(19) 0.73387(19) 0.11122(14) 0.0330(5) Uani 1 1 d . . .
N4 N 0.43797(19) 0.7785(2) 0.26443(14) 0.0360(6) Uani 1 1 d . . .
N5 N 0.2615(2) 0.6872(3) 0.27249(14) 0.0441(7) Uani 1 1 d . . .
C1 C 0.1999(3) 0.9861(3) 0.18386(19) 0.0441(8) Uani 1 1 d . . .
C2 C 0.2169(3) 1.0609(3) 0.2378(2) 0.0614(11) Uani 1 1 d . . .
H2A H 0.2645 1.0479 0.2808 0.074 Uiso 1 1 calc R . .
C3 C 0.1647(4) 1.1542(4) 0.2291(3) 0.0823(15) Uani 1 1 d . . .
H3A H 0.1779 1.2052 0.2660 0.099 Uiso 1 1 calc R . .
C4 C 0.0958(4) 1.1745(4) 0.1695(4) 0.0896(18) Uani 1 1 d . . .
H4A H 0.0609 1.2392 0.1643 0.108 Uiso 1 1 calc R . .
C5 C 0.0764(4) 1.1006(5) 0.1162(3) 0.0920(17) Uani 1 1 d . . .
H5A H 0.0269 1.1145 0.0743 0.110 Uiso 1 1 calc R . .
C6 C 0.1273(4) 1.0065(4) 0.1222(2) 0.0672(12) Uani 1 1 d . . .
H6A H 0.1132 0.9562 0.0848 0.081 Uiso 1 1 calc R . .
C7 C 0.2456(2) 0.6273(2) 0.06193(16) 0.0369(7) Uani 1 1 d . . .
C8 C 0.3435(2) 0.6595(2) 0.05900(15) 0.0333(6) Uani 1 1 d . . .
C9 C 0.3919(3) 0.6143(2) 0.00866(17) 0.0383(7) Uani 1 1 d . . .
H9A H 0.4593 0.6330 0.0083 0.046 Uiso 1 1 calc R . .
C10 C 0.3429(3) 0.5422(3) -0.04093(18) 0.0468(8) Uani 1 1 d . . .
H10A H 0.3764 0.5122 -0.0752 0.056 Uiso 1 1 calc R . .
C11 C 0.2455(3) 0.5144(3) -0.04009(19) 0.0535(9) Uani 1 1 d . . .
H11A H 0.2110 0.4669 -0.0749 0.064 Uiso 1 1 calc R . .
C12 C 0.1971(3) 0.5557(3) 0.01145(19) 0.0490(9) Uani 1 1 d . . .
H12A H 0.1304 0.5347 0.0122 0.059 Uiso 1 1 calc R . .
C13 C 0.0019(3) 0.6989(4) 0.0329(2) 0.0641(11) Uani 1 1 d . . .
H13A H 0.0123 0.7738 0.0265 0.096 Uiso 1 1 calc R . .
H13B H -0.0692 0.6858 0.0325 0.096 Uiso 1 1 calc R . .
H13C H 0.0220 0.6599 -0.0061 0.096 Uiso 1 1 calc R . .
C14 C 0.0394(3) 0.7409(4) 0.1887(2) 0.0678(12) Uani 1 1 d . . .
H14A H 0.0614 0.7099 0.2364 0.102 Uiso 1 1 calc R . .
H14B H -0.0338 0.7475 0.1780 0.102 Uiso 1 1 calc R . .
H14C H 0.0698 0.8102 0.1877 0.102 Uiso 1 1 calc R . .
C15 C 0.0471(3) 0.5174(4) 0.1397(2) 0.0694(13) Uani 1 1 d . . .
H15A H 0.0725 0.4699 0.1072 0.104 Uiso 1 1 calc R . .
H15B H -0.0259 0.5101 0.1327 0.104 Uiso 1 1 calc R . .
H15C H 0.0779 0.5000 0.1894 0.104 Uiso 1 1 calc R . .
C16 C 0.4698(3) 0.8514(3) -0.00029(19) 0.0511(9) Uani 1 1 d . . .
H16A H 0.4697 0.7897 -0.0308 0.077 Uiso 1 1 calc R . .
H16B H 0.5246 0.8982 -0.0061 0.077 Uiso 1 1 calc R . .
H16C H 0.4056 0.8882 -0.0142 0.077 Uiso 1 1 calc R . .
C17 C 0.4988(3) 0.9331(3) 0.1483(2) 0.0560(10) Uani 1 1 d . . .
H17A H 0.4318 0.9620 0.1470 0.084 Uiso 1 1 calc R . .
H17B H 0.5389 0.9835 0.1274 0.084 Uiso 1 1 calc R . .
H17C H 0.5316 0.9188 0.1980 0.084 Uiso 1 1 calc R . .
C18 C 0.6098(3) 0.7381(3) 0.1205(2) 0.0547(9) Uani 1 1 d . . .
H18A H 0.6242 0.7230 0.1720 0.082 Uiso 1 1 calc R . .
H18B H 0.6636 0.7816 0.1089 0.082 Uiso 1 1 calc R . .
H18C H 0.6057 0.6724 0.0936 0.082 Uiso 1 1 calc R . .
C19 C 0.4630(3) 0.8612(3) 0.30980(18) 0.0440(8) Uani 1 1 d . . .
H19A H 0.4185 0.9192 0.3052 0.053 Uiso 1 1 calc R . .
C20 C 0.5495(3) 0.8652(3) 0.36196(18) 0.0492(9) Uani 1 1 d . . .
H20A H 0.5632 0.9252 0.3918 0.059 Uiso 1 1 calc R . .
C21 C 0.6167(3) 0.7822(3) 0.37126(18) 0.0466(8) Uani 1 1 d . . .
C22 C 0.5900(3) 0.6969(3) 0.32662(18) 0.0447(8) Uani 1 1 d . . .
H22A H 0.6329 0.6376 0.3313 0.054 Uiso 1 1 calc R . .
C23 C 0.5030(2) 0.6967(3) 0.27589(17) 0.0401(7) Uani 1 1 d . . .
H23A H 0.4872 0.6360 0.2471 0.048 Uiso 1 1 calc R . .
C24 C 0.7121(3) 0.7845(4) 0.4275(2) 0.0689(12) Uani 1 1 d . . .
H24A H 0.6957 0.7942 0.4748 0.103 Uiso 1 1 calc R . .
H24B H 0.7544 0.8424 0.4176 0.103 Uiso 1 1 calc R . .
H24C H 0.7481 0.7184 0.4266 0.103 Uiso 1 1 calc R . .
C25 C 0.2397(3) 0.7369(4) 0.3315(2) 0.0651(12) Uani 1 1 d . . .
H25A H 0.2406 0.8112 0.3327 0.078 Uiso 1 1 calc R . .
C26 C 0.2168(4) 0.6846(6) 0.3883(2) 0.0924(19) Uani 1 1 d . . .
H26A H 0.2001 0.7226 0.4271 0.111 Uiso 1 1 calc R . .
C27 C 0.2176(4) 0.5761(7) 0.3900(3) 0.108(3) Uani 1 1 d . . .
C28 C 0.2413(3) 0.5262(5) 0.3322(3) 0.0886(18) Uani 1 1 d . . .
H28A H 0.2426 0.4519 0.3314 0.106 Uiso 1 1 calc R . .
C29 C 0.2635(3) 0.5814(3) 0.2750(2) 0.0581(10) Uani 1 1 d . . .
H29A H 0.2807 0.5438 0.2362 0.070 Uiso 1 1 calc R . .
C30 C 0.1954(5) 0.5160(8) 0.4543(4) 0.179(4) Uani 1 1 d . . .
H30A H 0.2308 0.4488 0.4586 0.269 Uiso 1 1 calc R . .
H30B H 0.1231 0.5037 0.4476 0.269 Uiso 1 1 calc R . .
H30C H 0.2183 0.5570 0.4981 0.269 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'
Si Si 0.0817 0.0704 '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 W N3 119.86(11) . . ?
N1 W N2 111.59(12) . . ?
N3 W N2 78.34(10) . . ?
N1 W N5 103.81(12) . . ?
N3 W N5 136.30(11) . . ?
N2 W N5 87.91(10) . . ?
N1 W N4 101.58(12) . . ?
N3 W N4 88.80(10) . . ?
N2 W N4 146.60(10) . . ?
N5 W N4 80.33(10) . . ?
N2 Si1 C14 112.04(16) . . ?
N2 Si1 C13 109.50(17) . . ?
C14 Si1 C13 105.0(2) . . ?
N2 Si1 C15 112.21(18) . . ?
C14 Si1 C15 107.6(2) . . ?
C13 Si1 C15 110.2(2) . . ?
N3 Si2 C17 111.07(14) . . ?
N3 Si2 C18 112.27(15) . . ?
C17 Si2 C18 107.94(19) . . ?
N3 Si2 C16 111.62(15) . . ?
C17 Si2 C16 105.18(18) . . ?
C18 Si2 C16 108.44(18) . . ?
C1 N1 W 169.7(3) . . ?
C7 N2 Si1 119.7(2) . . ?
C7 N2 W 115.66(19) . . ?
Si1 N2 W 124.03(14) . . ?
C8 N3 Si2 118.4(2) . . ?
C8 N3 W 115.54(19) . . ?
Si2 N3 W 124.58(13) . . ?
C23 N4 C19 115.1(3) . . ?
C23 N4 W 120.3(2) . . ?
C19 N4 W 124.4(2) . . ?
C29 N5 C25 116.0(3) . . ?
C29 N5 W 120.6(2) . . ?
C25 N5 W 123.1(3) . . ?
C2 C1 N1 120.7(3) . . ?
C2 C1 C6 118.5(4) . . ?
N1 C1 C6 120.8(3) . . ?
C3 C2 C1 120.1(4) . . ?
C4 C3 C2 121.5(5) . . ?
C3 C4 C5 119.3(5) . . ?
C4 C5 C6 121.3(5) . . ?
C5 C6 C1 119.3(5) . . ?
C12 C7 C8 119.0(3) . . ?
C12 C7 N2 126.1(3) . . ?
C8 C7 N2 114.9(3) . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 N3 125.5(3) . . ?
C7 C8 N3 115.1(3) . . ?
C10 C9 C8 120.9(3) . . ?
C11 C10 C9 119.6(3) . . ?
C10 C11 C12 120.4(3) . . ?
C11 C12 C7 120.7(3) . . ?
N4 C19 C20 123.5(3) . . ?
C19 C20 C21 120.5(3) . . ?
C22 C21 C20 116.0(3) . . ?
C22 C21 C24 122.2(4) . . ?
C20 C21 C24 121.7(3) . . ?
C23 C22 C21 121.1(3) . . ?
N4 C23 C22 123.6(3) . . ?
C26 C25 N5 123.0(5) . . ?
C25 C26 C27 120.5(5) . . ?
C28 C27 C26 116.8(5) . . ?
C28 C27 C30 121.9(8) . . ?
C26 C27 C30 121.3(7) . . ?
C27 C28 C29 121.5(6) . . ?
N5 C29 C28 122.2(5) . . ?
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
W N1 1.753(3) . ?
W N3 2.060(2) . ?
W N2 2.062(3) . ?
W N5 2.083(3) . ?
W N4 2.109(3) . ?
Si1 N2 1.754(3) . ?
Si1 C14 1.863(4) . ?
Si1 C13 1.865(4) . ?
Si1 C15 1.872(4) . ?
Si2 N3 1.761(3) . ?
Si2 C17 1.858(4) . ?
Si2 C18 1.872(4) . ?
Si2 C16 1.877(4) . ?
N1 C1 1.390(4) . ?
N2 C7 1.413(4) . ?
N3 C8 1.413(4) . ?
N4 C23 1.359(4) . ?
N4 C19 1.365(4) . ?
N5 C29 1.354(5) . ?
N5 C25 1.376(5) . ?
C1 C2 1.389(5) . ?
C1 C6 1.398(5) . ?
C2 C3 1.381(6) . ?
C3 C4 1.343(8) . ?
C4 C5 1.373(8) . ?
C5 C6 1.383(7) . ?
C7 C12 1.393(4) . ?
C7 C8 1.407(4) . ?
C8 C9 1.394(4) . ?
C9 C10 1.390(5) . ?
C10 C11 1.376(5) . ?
C11 C12 1.392(5) . ?
C19 C20 1.378(5) . ?
C20 C21 1.390(5) . ?
C21 C22 1.385(5) . ?
C21 C24 1.506(5) . ?
C22 C23 1.369(5) . ?
C25 C26 1.362(6) . ?
C26 C27 1.389(9) . ?
C27 C28 1.366(9) . ?
C27 C30 1.527(7) . ?
C28 C29 1.382(5) . ?
