#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/75/2007556.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007556
loop_
_publ_author_name
'Wang, Shu-Yu S.'
'Boncella, James M.'
'Abboud, Khalil A.'
_publ_section_title
;[N,N'-Bis(trimethylsilyl)-o-phenylenediamido](1,4-butanediyl)(phenylimido)tungsten(VI),
 a Deactivation Product from Olefin Metathesis Polymerization
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800035
_journal_paper_doi               10.1107/S010827019809948X
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[W (C4 H8) (C6 H5 N) (C12 H22 N2 Si2 )]'
_chemical_formula_sum            'C22 H35 N3 Si2 W'
_chemical_formula_weight         581.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.4710(10)
_cell_angle_beta                 97.9540(10)
_cell_angle_gamma                102.2470(10)
_cell_formula_units_Z            2
_cell_length_a                   9.21180(10)
_cell_length_b                   12.0569(2)
_cell_length_c                   12.0845(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1243.77(3)
_computing_cell_refinement       'Siemens SMART & SAINT, (Siemens, 1995)'
_computing_data_collection       'Siemens SMART, (Siemens, 1995)'
_computing_data_reduction        'Siemens SHELXTL5, (Sheldrick, 1995)'
_computing_molecular_graphics    'Siemens SHELX-97'
_computing_publication_material  'Siemens SHELX-97'
_computing_structure_refinement  'Siemens SHELX-97'
_computing_structure_solution    'Siemens SHELX-97, (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'Siemens SMART platform / CCD'
_diffrn_measurement_method       ω
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8213
_diffrn_reflns_theta_full        20.80
_diffrn_reflns_theta_max         26.92
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        '< 1'
_exptl_absorpt_coefficient_mu    4.752
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS, Blessing 1995)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.78
_refine_ls_extinction_coef       0.0010(2)
_refine_ls_extinction_method     SHELX-97
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4600
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_obs          .0244
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0250P)²+0.5695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .0564
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                4204
_reflns_number_total             4600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            qb0044.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.5695P] 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^)+(0.0250P)^2^+0.5695P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2007556
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
W .19059(2) .699360(10) .797140(10) .02675(7) Uani d . 1 . . W
Si1 -.18060(10) .58830(10) .80470(10) .0350(3) Uani d . 1 . . Si
Si2 .28580(10) .84190(10) .59360(10) .0335(2) Uani d . 1 . . Si
N1 -.0276(4) .6972(3) .7931(3) .0298(7) Uani d . 1 . . N
N2 .1807(4) .8106(3) .6984(3) .0299(7) Uani d . 1 . . N
N3 .2267(4) .5638(3) .7369(3) .0319(7) Uani d . 1 . . N
C1 .2030(4) .6996(4) .9784(3) .0393(10) Uani d D 1 . . C
H1A .1417 .6260 .9820 .047 Uiso d PR .61(2) A 1 H
H1B .1651 .7628 1.0196 .047 Uiso d PR .61(2) A 1 H
H1C .1811 .6187 .9804 .047 Uiso d PR .39(2) A 2 H
H1D .1246 .7327 1.0068 .047 Uiso d PR .39(2) A 2 H
C2 .3695(7) .7165(9) 1.0357(12) .049(3) Uani d PD .61(2) A 1 C
H2A .3790 .7248 1.1185 .059 Uiso calc PR .61(2) A 1 H
H2B .4057 .6488 1.0001 .059 Uiso calc PR .61(2) A 1 H
C3 .4591(13) .8269(9) 1.0165(4) .043(3) Uani d PD .61(2) A 1 C
H3A .5669 .8352 1.0391 .052 Uiso calc PR .61(2) A 1 H
H3B .4344 .8962 1.0623 .052 Uiso calc PR .61(2) A 1 H
C2' .3555(9) .764(3) 1.0639(11) .063(7) Uani d PD .39(2) A 2 C
H2'A .3540 .8424 1.1076 .075 Uiso calc PR .39(2) A 2 H
H2'B .3772 .7193 1.1184 .075 Uiso calc PR .39(2) A 2 H
C3' .4713(17) .770(2) .9883(13) .048(5) Uani d PD .39(2) A 2 C
H3'A .4879 .6916 .9591 .057 Uiso calc PR .39(2) A 2 H
H3'B .5669 .8230 1.0339 .057 Uiso calc PR .39(2) A 2 H
C4 .4156(5) .8138(4) .8852(3) .0385(10) Uani d D 1 . . C
H4A .4212 .8911 .8754 .046 Uiso d PR .61(2) A 1 H
H4B .4894 .7831 .8470 .046 Uiso d PR .61(2) A 1 H
H4C .4100 .8944 .9126 .046 Uiso d PR .39(2) A 2 H
H4D .4837 .8104 .8318 .046 Uiso d PR .39(2) A 2 H
C5 -.0238(4) .8156(4) .8017(3) .0312(8) Uani d . 1 . . C
C6 .0883(4) .8761(3) .7510(3) .0317(9) Uani d . 1 . . C
C7 .0957(5) .9958(4) .7563(4) .0420(10) Uani d . 1 . . C
H7A .1697 1.0374 .7260 .050 Uiso calc R 1 . . H
C8 -.0056(6) 1.0513(4) .8056(4) .0510(12) Uani d . 1 . . C
H8A -.0008 1.1294 .8066 .061 Uiso calc R 1 . . H
C9 -.1147(6) .9923(4) .8539(4) .0516(12) Uani d . 1 . . C
H9A -.1828 1.0308 .8865 .062 Uiso calc R 1 . . H
C10 -.1228(5) .8771(4) .8539(4) .0422(10) Uani d . 1 . . C
H10A -.1944 .8393 .8887 .051 Uiso calc R 1 . . H
C11 .2430(4) .4516(3) .6871(3) .0286(8) Uani d . 1 . . C
C12 .3125(5) .3929(4) .7549(4) .0370(9) Uani d . 1 . . C
H12A .3479 .4288 .8346 .044 Uiso calc R 1 . . H
C13 .3297(5) .2812(4) .7052(4) .0438(11) Uani d . 1 . . C
H13A .3754 .2422 .7518 .053 Uiso calc R 1 . . H
C14 .2797(5) .2274(4) .5874(4) .0435(11) Uani d . 1 . . C
H14A .2938 .1531 .5540 .052 Uiso calc R 1 . . H
C15 .2092(5) .2836(4) .5195(4) .0443(11) Uani d . 1 . . C
H15A .1737 .2466 .4400 .053 Uiso calc R 1 . . H
C16 .1901(5) .3953(4) .5681(3) .0364(9) Uani d . 1 . . C
H16A .1420 .4328 .5212 .044 Uiso calc R 1 . . H
C17 -.2160(6) .6169(5) .9569(4) .0544(13) Uani d . 1 . . C
H17A -.1267 .6185 1.0093 .082 Uiso calc R 1 . . H
H17B -.2991 .5552 .9599 .082 Uiso calc R 1 . . H
H17C -.2404 .6919 .9796 .082 Uiso calc R 1 . . H
C18 -.1266(5) .4455(4) .7660(4) .0435(10) Uani d . 1 . . C
H18A -.0375 .4501 .8205 .065 Uiso calc R 1 . . H
H18B -.1060 .4299 .6886 .065 Uiso calc R 1 . . H
H18C -.2083 .3826 .7690 .065 Uiso calc R 1 . . H
C19 -.3520(5) .5851(5) .7027(4) .0482(11) Uani d . 1 . . C
H19A -.3766 .6600 .7251 .072 Uiso calc R 1 . . H
H19B -.4353 .5232 .7052 .072 Uiso calc R 1 . . H
H19C -.3329 .5705 .6249 .072 Uiso calc R 1 . . H
C20 .4557(5) .9700(4) .6602(4) .0504(12) Uani d . 1 . . C
H20A .5180 .9536 .7216 .076 Uiso calc R 1 . . H
H20B .4236 1.0400 .6917 .076 Uiso calc R 1 . . H
H20C .5128 .9821 .6017 .076 Uiso calc R 1 . . H
C21 .3517(5) .7079(4) .5358(4) .0450(11) Uani d . 1 . . C
H21A .4148 .6935 .5982 .068 Uiso calc R 1 . . H
H21B .4089 .7198 .4772 .068 Uiso calc R 1 . . H
H21C .2657 .6409 .5021 .068 Uiso calc R 1 . . H
C22 .1634(5) .8716(4) .4747(4) .0440(11) Uani d . 1 . . C
H22A .1301 .9411 .5058 .066 Uiso calc R 1 . . H
H22B .0768 .8050 .4409 .066 Uiso calc R 1 . . H
H22C .2199 .8839 .4159 .066 Uiso calc R 1 . . H
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_publ_flag
N3 W N1 115.78(15) yes
N3 W N2 118.68(13) yes
N1 W N2 83.56(12) yes
N3 W C1 100.89(16) yes
N1 W C1 86.18(13) yes
N2 W C1 139.67(15) yes
N3 W C4 103.33(16) yes
N1 W C4 139.50(15) yes
N2 W C4 86.87(14) yes
C1 W C4 76.18(16) yes
N1 Si1 C19 108.62(19) ?
N1 Si1 C18 106.43(18) ?
C19 Si1 C18 111.6(2) ?
N1 Si1 C17 112.0(2) ?
C19 Si1 C17 109.9(2) ?
C18 Si1 C17 108.2(2) ?
N2 Si2 C21 105.97(18) ?
N2 Si2 C22 110.10(18) ?
C21 Si2 C22 110.4(2) ?
N2 Si2 C20 111.69(19) ?
C21 Si2 C20 108.4(2) ?
C22 Si2 C20 110.3(2) ?
C5 N1 Si1 126.7(3) ?
C5 N1 W 101.2(2) ?
Si1 N1 W 131.06(17) ?
C6 N2 Si2 126.8(3) ?
C6 N2 W 100.8(2) ?
Si2 N2 W 131.34(17) ?
C11 N3 W 175.4(3) ?
C2' C1 C2 23.7(8) ?
C2' C1 W 117.3(8) ?
C2 C1 W 109.1(6) ?
C2' C1 H1A 122.0 ?
C2 C1 H1A 110.1 ?
W C1 H1A 109.7 ?
C2' C1 H1B 86.1 ?
C2 C1 H1B 109.7 ?
W C1 H1B 109.9 ?
H1A C1 H1B 108.2 ?
C2' C1 H1C 106.3 ?
C2 C1 H1C 89.4 ?
W C1 H1C 108.0 ?
H1A C1 H1C 23.6 ?
H1B C1 H1C 128.1 ?
C2' C1 H1D 109.2 ?
C2 C1 H1D 131.4 ?
W C1 H1D 108.2 ?
H1A C1 H1D 84.8 ?
H1B C1 H1D 26.5 ?
H1C C1 H1D 107.3 ?
C3 C2 C1 106.6(6) ?
C3 C2 H2A 110.4 ?
C1 C2 H2A 110.4 ?
C3 C2 H2B 110.4 ?
C1 C2 H2B 110.4 ?
H2A C2 H2B 108.6 ?
C2 C3 C4 106.5(8) ?
C2 C3 H3A 110.4 ?
C4 C3 H3A 110.4 ?
C2 C3 H3B 110.4 ?
C4 C3 H3B 110.4 ?
H3A C3 H3B 108.6 ?
C3' C2' C1 105.0(10) ?
C3' C2' H2'A 110.7 ?
C1 C2' H2'A 110.7 ?
C3' C2' H2'B 110.7 ?
C1 C2' H2'B 110.7 ?
H2'A C2' H2'B 108.8 ?
C2' C3' C4 109.7(14) ?
C2' C3' H3'A 109.7 ?
C4 C3' H3'A 109.7 ?
C2' C3' H3'B 109.7 ?
C4 C3' H3'B 109.7 ?
H3'A C3' H3'B 108.2 ?
C3' C4 C3 27.4(6) ?
C3' C4 W 107.6(8) ?
C3 C4 W 115.4(4) ?
C3' C4 H4A 133.6 ?
C3 C4 H4A 108.6 ?
W C4 H4A 108.4 ?
C3' C4 H4B 87.7 ?
C3 C4 H4B 108.4 ?
W C4 H4B 108.4 ?
H4A C4 H4B 107.4 ?
C3' C4 H4C 110.5 ?
C3 C4 H4C 83.3 ?
W C4 H4C 109.9 ?
H4A C4 H4C 28.3 ?
H4B C4 H4C 129.3 ?
C3' C4 H4D 110.6 ?
C3 C4 H4D 125.3 ?
W C4 H4D 110.0 ?
H4A C4 H4D 83.1 ?
H4B C4 H4D 25.5 ?
H4C C4 H4D 108.3 ?
N1 C5 C10 124.9(4) ?
N1 C5 C6 116.2(3) ?
C10 C5 C6 118.9(4) ?
N2 C6 C7 125.1(4) ?
N2 C6 C5 116.5(3) ?
C7 C6 C5 118.4(4) ?
C8 C7 C6 120.7(4) ?
C8 C7 H7A 119.7 ?
C6 C7 H7A 119.7 ?
C7 C8 C9 120.9(4) ?
C7 C8 H8A 119.6 ?
C9 C8 H8A 119.6 ?
C10 C9 C8 120.4(4) ?
C10 C9 H9A 119.8 ?
C8 C9 H9A 119.8 ?
C9 C10 C5 120.8(4) ?
C9 C10 H10A 119.6 ?
C5 C10 H10A 119.6 ?
N3 C11 C12 120.5(3) ?
N3 C11 C16 121.0(3) ?
C12 C11 C16 118.6(4) ?
C13 C12 C11 120.6(4) ?
C13 C12 H12A 119.7 ?
C11 C12 H12A 119.7 ?
C14 C13 C12 120.4(4) ?
C14 C13 H13A 119.8 ?
C12 C13 H13A 119.8 ?
C15 C14 C13 119.7(4) ?
C15 C14 H14A 120.1 ?
C13 C14 H14A 120.1 ?
C14 C15 C16 120.6(4) ?
C14 C15 H15A 119.7 ?
C16 C15 H15A 119.7 ?
C15 C16 C11 120.2(4) ?
C15 C16 H16A 119.9 ?
C11 C16 H16A 119.9 ?
Si1 C17 H17A 109.5 ?
Si1 C17 H17B 109.5 ?
H17A C17 H17B 109.5 ?
Si1 C17 H17C 109.5 ?
H17A C17 H17C 109.5 ?
H17B C17 H17C 109.5 ?
Si1 C18 H18A 109.5 ?
Si1 C18 H18B 109.5 ?
H18A C18 H18B 109.5 ?
Si1 C18 H18C 109.5 ?
H18A C18 H18C 109.5 ?
H18B C18 H18C 109.5 ?
Si1 C19 H19A 109.5 ?
Si1 C19 H19B 109.5 ?
H19A C19 H19B 109.5 ?
Si1 C19 H19C 109.5 ?
H19A C19 H19C 109.5 ?
H19B C19 H19C 109.5 ?
Si2 C20 H20A 109.5 ?
Si2 C20 H20B 109.5 ?
H20A C20 H20B 109.5 ?
Si2 C20 H20C 109.5 ?
H20A C20 H20C 109.5 ?
H20B C20 H20C 109.5 ?
Si2 C21 H21A 109.5 ?
Si2 C21 H21B 109.5 ?
H21A C21 H21B 109.5 ?
Si2 C21 H21C 109.5 ?
H21A C21 H21C 109.5 ?
H21B C21 H21C 109.5 ?
Si2 C22 H22A 109.5 ?
Si2 C22 H22B 109.5 ?
H22A C22 H22B 109.5 ?
Si2 C22 H22C 109.5 ?
H22A C22 H22C 109.5 ?
H22B C22 H22C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W N3 . 1.736(3) yes
W N1 . 1.998(3) yes
W N2 . 2.013(3) yes
W C1 . 2.177(4) yes
W C4 . 2.185(4) yes
Si1 N1 . 1.758(3) ?
Si1 C19 . 1.851(4) ?
Si1 C18 . 1.859(5) ?
Si1 C17 . 1.873(4) ?
Si2 N2 . 1.762(3) ?
Si2 C21 . 1.854(4) ?
Si2 C22 . 1.856(4) ?
Si2 C20 . 1.867(5) ?
N1 C5 . 1.398(5) ?
N2 C6 . 1.392(5) ?
N3 C11 . 1.385(5) ?
C1 C2' . 1.541(5) ?
C1 C2 . 1.541(5) ?
C1 H1A . .9600 ?
C1 H1B . .9600 ?
C1 H1C . .9600 ?
C1 H1D . .9600 ?
C2 C3 . 1.499(9) ?
C2 H2A . .9700 ?
C2 H2B . .9700 ?
C3 C4 . 1.541(5) ?
C3 H3A . .9700 ?
C3 H3B . .9700 ?
C2' C3' . 1.499(9) ?
C2' H2'A . .9700 ?
C2' H2'B . .9700 ?
C3' C4 . 1.541(5) ?
C3' H3'A . .9700 ?
C3' H3'B . .9700 ?
C4 H4A . .9600 ?
C4 H4B . .9600 ?
C4 H4C . .9600 ?
C4 H4D . .9600 ?
C5 C10 . 1.412(5) ?
C5 C6 . 1.433(5) ?
C6 C7 . 1.415(6) ?
C7 C8 . 1.376(6) ?
C7 H7A . .9300 ?
C8 C9 . 1.387(7) ?
C8 H8A . .9300 ?
C9 C10 . 1.374(6) ?
C9 H9A . .9300 ?
C10 H10A . .9300 ?
C11 C12 . 1.386(5) ?
C11 C16 . 1.395(5) ?
C12 C13 . 1.382(6) ?
C12 H12A . .9300 ?
C13 C14 . 1.375(6) ?
C13 H13A . .9300 ?
C14 C15 . 1.368(6) ?
C14 H14A . .9300 ?
C15 C16 . 1.386(6) ?
C15 H15A . .9300 ?
C16 H16A . .9300 ?
C17 H17A . .9600 ?
C17 H17B . .9600 ?
C17 H17C . .9600 ?
C18 H18A . .9600 ?
C18 H18B . .9600 ?
C18 H18C . .9600 ?
C19 H19A . .9600 ?
C19 H19B . .9600 ?
C19 H19C . .9600 ?
C20 H20A . .9600 ?
C20 H20B . .9600 ?
C20 H20C . .9600 ?
C21 H21A . .9600 ?
C21 H21B . .9600 ?
C21 H21C . .9600 ?
C22 H22A . .9600 ?
C22 H22B . .9600 ?
C22 H22C . .9600 ?
