#------------------------------------------------------------------------------
#$Date: 2017-01-26 16:57:48 +0200 (Thu, 26 Jan 2017) $
#$Revision: 190984 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/33/2003331.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_2003331
loop_
_publ_author_name
'Evans, S. V.'
'Legzdins, P.'
'Rettig, S. J.'
'Sánchez, L.'
'Trotter, J.'
_publ_section_title
;
 A Tungsten Nitrosyl Complex
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              584
_journal_page_last               586
_journal_paper_doi               10.1107/S0108270194010942
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
;
Synthesis (Legzdins, Rettig & Sánchez, 1988)
;
_chemical_formula_moiety         'C13 H27 N3 O3 Si2 W'
_chemical_formula_structural
;
(C5 H5) W (N O) (O N (C H2 Si (C H3)3) N O) (C H2 Si (C H3)3)
;
_chemical_formula_sum            'C13 H27 N3 O3 Si2 W'
_chemical_formula_weight         513.40
_chemical_name_systematic
;
(η⁵-Cyclopentadienyl)nitrosyl(trimethylsilylmethyl)
(N-trimethylsilylmethyl-N-nitrosohydroxylaminato)tungsten
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                111.51(2)
_cell_angle_beta                 107.92(2)
_cell_angle_gamma                94.07(2)
_cell_formula_units_Z            4
_cell_length_a                   12.610(3)
_cell_length_b                   16.038(4)
_cell_length_c                   12.106(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     2120.1(10)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'local program'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'ORFLS (Busing, Martin & Levy, 1962)'
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Enraf-Nonius CAD-4F'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Molybdenum K\a~1~'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6228
_diffrn_reflns_theta_max         26.25
_diffrn_standards_decay_%        68
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.6
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.1
_refine_diff_density_min         -1.9
_refine_ls_goodness_of_fit_obs   1.54
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     327
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .050
_refine_ls_shift/esd_max         .13
_refine_ls_shift/esd_mean        .02
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/σ²(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .046
_reflns_number_observed          2442
_reflns_number_total             6228
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            cr1148.cif
_cod_data_source_block           structure
_cod_depositor_comments
;
 Adding the _atom_site_type_symbol data item.

 Antanas Vaitkus,
 2017-01-26

 Marking atoms 'Cp' and 'Cp'' as dummy atoms.

 Antanas Vaitkus,
 2017-01-26

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/\s^2^(F)' 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^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2120.0(10)
_cod_database_code               2003331
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_calc_flag
W W .11916(7) .22523(6) .02029(8) .052 d
Si(1) Si .2005(6) .0828(5) -.2302(6) .082 d
Si(2) Si .3393(5) .0534(5) .2734(6) .078 d
N(1) N -.0039(14) .1872(12) -.1172(17) .059 d
N(2) N .1436(15) .0797(13) .1086(16) .065(5) d
N(3) N .0628(13) .1024(14) .1400(17) .070 d
O(1) O -.0949(14) .1711(12) -.2047(15) .100 d
O(2) O .1917(10) .1179(10) .0539(11) .068 d
O(3) O .0251(9) .1655(11) .1032(12) .059 d
C(1) C .2275(15) .1970(14) -.0944(18) .060 d
C(2) C .2595(15) .3629(15) .1188(18) .060(6) d
C(3) C .1506(17) .3742(16) .052(2) .074(7) d
C(4) C .0782(16) .3660(15) .1161(19) .066(6) d
C(5) C .1461(19) .3463(17) .218(2) .084(7) d
C(6) C .2518(16) .3485(16) .215(2) .074(7) d
Cp . .1772 .3596 .1440 .07 dum
C(7) C .061(3) .014(3) -.307(4) .251 d
C(8) C .259(6) .094(2) -.340(4) .350 d
C(9) C .264(5) .000(3) -.170(3) .264 d
C(10) C .1900(17) .0061(18) .139(2) .085(7) d
C(11) C .444(2) .088(3) .211(3) .173 d
C(12) C .377(2) -.039(2) .325(2) .127 d
C(13) C .327(3) .155(2) .400(2) .152 d
W' W .74095(7) .36181(7) .17686(8) .057 d
Si(1)' Si .6126(6) .5457(5) .2845(7) .088 d
Si(2)' Si .8466(7) .3260(5) .6215(7) .090 d
N(1)' N .7875(19) .4431(19) .1432(18) .108 d
N(2)' N .8605(16) .4027(13) .4512(17) .069(5) d
N(3)' N .9378(15) .3891(15) .4110(19) .094 d
O(1)' O .831(2) .4988(15) .1083(19) .149 d
O(2)' O .7541(11) .3960(9) .3683(12) .066 d
O(3)' O .9088(10) .3691(12) .2900(15) .085 d
C(1)' C .5914(16) .4205(16) .1894(18) .075 d
C(2)' C .5881(19) .2396(18) .023(2) .092(5) d
C(3)' C .6560(19) .2636(17) -.0387(21) .086(7) d
C(4)' C .7598(16) .2412(16) .012(2) .070(6) d
C(5)' C .757(2) .2057(18) .092(2) .095(8) d
C(6)' C .651(2) .2017(18) .099(2) .092(8) d
Cp' . .6824 .2304 .0373 .09 dum
C(7)' C .747(2) .604(2) .418(3) .156 d
C(8)' C .595(5) .604(3) .181(3) .320 d
C(9)' C .498(3) .567(3) .344(6) .380 d
C(10)' C .8715(16) .4277(16) .584(2) .075(7) d
C(11)' C .725(4) .251(3) .517(3) .272 d
C(12)' C .849(2) .3697(17) .785(2) .107 d
C(13)' C .974(3) .268(3) .608(4) .232 d
H(1a) H .2241 .2429 -.1303 .07 ?
H(1b) H .3052 .2068 -.0352 .07 ?
H(2) H .3269 .3655 .0965 .07 ?
H(3) H .1305 .3855 -.0243 .09 ?
H(4) H -.0007 .3725 .0959 .08 ?
H(5) H .1202 .3333 .2785 .10 ?
H(6) H .3149 .3403 .2778 .09 ?
H(7a) H .0600 -.0430 -.3751 .30 ?
H(7b) H .0371 -.0003 -.2447 .30 ?
H(7c) H .0080 .0474 -.3426 .30 ?
H(8a) H .2440 .0339 -.4098 .42 ?
H(8b) H .2236 .1364 -.3732 .42 ?
H(8c) H .3411 .1176 -.2970 .42 ?
H(9a) H .2493 -.0591 -.2409 .32 ?
H(9b) H .3462 .0233 -.1251 .32 ?
H(9c) H .2294 -.0072 -.1104 .32 ?
H(10a) H .1966 -.0397 .0622 .10 ?
H(10b) H .1380 -.0229 .1662 .10 ?
H(11a) H .5193 .1114 .2785 .21 ?
H(11b) H .4468 .0340 .1398 .21 ?
H(11c) H .4209 .1350 .1813 .21 ?
H(12a) H .4525 -.0170 .3928 .15 ?
H(12b) H .3205 -.0567 .3561 .15 ?
H(12c) H .3794 -.0919 .2524 .15 ?
H(13a) H .4003 .1808 .4705 .18 ?
H(13b) H .3035 .2001 .3667 .18 ?
H(13c) H .2693 .1365 .4310 .18 ?
H(1a)' H .5415 .4072 .1024 .09 ?
H(1b)' H .5526 .3887 .2262 .09 ?
H(2)' H .5110 .2485 .0133 .10 ?
H(3)' H .6354 .2896 -.1012 .10 ?
H(4)' H .8259 .2508 -.0107 .08 ?
H(5)' H .8195 .1856 .1382 .11 ?
H(6)' H .6247 .1763 .1499 .11 ?
H(7a)' H .7466 .6689 .4594 .19 ?
H(7b)' H .7561 .5763 .4799 .19 ?
H(7c)' H .8105 .5973 .3872 .19 ?
H(8a)' H .6053 .6704 .2311 .38 ?
H(8b)' H .6500 .5934 .1389 .38 ?
H(8c)' H .5170 .5817 .1168 .38 ?
H(9a)' H .5087 .6332 .3939 .46 ?
H(9b)' H .4249 .5461 .2722 .46 ?
H(9c)' H .4972 .5344 .3978 .46 ?
H(10a)' H .8157 .4653 .6011 .09 ?
H(10b)' H .9485 .4637 .6385 .09 ?
H(11a)' H .7154 .1994 .5401 .33 ?
H(11b)' H .6604 .2816 .5184 .33 ?
H(11c)' H .7281 .2288 .4312 .33 ?
H(12a)' H .8365 .3183 .8080 .13 ?
H(12b)' H .9235 .4097 .8430 .13 ?
H(12c)' H .7891 .4047 .7917 .13 ?
H(13a)' H .9673 .2135 .6264 .28 ?
H(13b)' H .9747 .2492 .5212 .28 ?
H(13c)' H 1.0457 .3109 .6686 .28 ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
? ? 'International Tables for X-ray Crystallography (1974, Vol. IV)' ? ?
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
N(1) W O(2) 113.7(6) yes
N(1) W O(3) 88.3(6) yes
N(1) W C(1) 91.1(7) yes
N(1) W Cp 122.7 yes
O(2) W O(3) 70.3(5) yes
O(2) W C(1) 76.6(6) yes
O(2) W Cp 123.4 yes
O(3) W C(1) 143.4(7) yes
O(3) W Cp 105.2 yes
C(1) W Cp 105.8 yes
C(1) Si(1) C(7) 118.8(12) no
C(1) Si(1) C(8) 110.5(13) no
C(1) Si(1) C(9) 110.0(13) no
C(7) Si(1) C(8) 112(2) no
C(7) Si(1) C(9) 95(2) no
C(8) Si(1) C(9) 110(2) no
C(10) Si(2) C(11) 109.1(11) no
C(10) Si(2) C(12) 107.5(11) no
C(10) Si(2) C(13) 106.6(12) no
C(11) Si(2) C(12) 110.6(15) no
C(11) Si(2) C(13) 110(2) no
C(12) Si(2) C(13) 113.1(13) no
W N(1) O(1) 171(2) yes
N(3) N(2) O(2) 124(2) yes
N(3) N(2) C(10) 117(2) yes
O(2) N(2) C(10) 118(2) yes
N(2) N(3) O(3) 112(2) yes
W O(2) N(2) 114.5(12) yes
W O(3) N(3) 118.6(10) yes
W C(1) Si(1) 121.6(10) yes
C(3) C(2) C(6) 107(2) no
C(2) C(3) C(4) 108(2) no
C(3) C(4) C(5) 104(2) no
C(4) C(5) C(6) 108(2) no
C(2) C(6) C(5) 112(2) no
Si(2) C(10) N(2) 111(2) yes
N(1)' W' O(2)' 117.5(8) yes
N(1)' W' O(3)' 89.7(9) yes
N(1)' W' C(1)' 90.0(9) yes
N(1)' W' Cp' 119.2 yes
O(2)' W' O(3)' 69.7(5) yes
O(2)' W' C(1)' 76.0(6) yes
O(2)' W' Cp' 123.2 yes
O(3)' W' C(1)' 141.0(7) yes
O(3)' W' Cp' 106.9 yes
C(1)' W' Cp' 107.1 yes
C(1)' Si(1)' C(7)' 118.3(12) no
C(1)' Si(1)' C(8)' 109.4(14) no
C(1)' Si(1)' C(9)' 109.3(13) no
C(7)' Si(1)' C(8)' 108(2) no
C(7)' Si(1)' C(9)' 108(2) no
C(8)' Si(1)' C(9)' 103(2) no
C(10)' Si(2)' C(11)' 112(2) no
C(10)' Si(2)' C(12)' 107.4(11) no
C(10)' Si(2)' C(13)' 104.7(13) no
C(11)' Si(2)' C(12)' 112.5(14) no
C(11)' Si(2)' C(13)' 109(2) no
C(12)' Si(2)' C(13)' 110.9(15) no
W' N(1)' O(1)' 172(2) yes
N(3)' N(2)' O(2)' 119(2) yes
N(3)' N(2)' C(10)' 125(2) yes
O(2)' N(2)' C(10)' 116(2) yes
N(2)' N(3)' O(3)' 114(2) yes
W' O(2)' N(2)' 115.4(10) yes
W' O(3)' N(3)' 121.6(11) yes
W' C(1)' Si(1)' 118.7(9) yes
C(3)' C(2)' C(6)' 108(2) no
C(2)' C(3)' C(4)' 104(2) no
C(3)' C(4)' C(5)' 112(2) no
C(4)' C(5)' C(6)' 108(2) no
C(2)' C(6)' C(5)' 108(2) no
Si(2)' C(10)' N(2)' 113(2) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
W N(1) 1.76(2) yes
W O(2) 2.12(2) yes
W O(3) 2.150(10) yes
W C(1) 2.19(2) yes
W C(2) 2.38(2) yes
W C(3) 2.26(2) yes
W C(4) 2.31(2) yes
W C(5) 2.37(2) yes
W C(6) 2.44(2) yes
W Cp 2.04 yes
Si(1) C(1) 1.88(2) yes
Si(1) C(7) 1.78(3) no
Si(1) C(8) 1.75(3) no
Si(1) C(9) 1.85(3) no
Si(2) C(10) 1.94(2) yes
Si(2) C(11) 1.85(2) no
Si(2) C(12) 1.84(3) no
Si(2) C(13) 1.84(3) no
N(1) O(1) 1.23(2) yes
N(2) N(3) 1.23(2) yes
N(2) O(2) 1.29(2) yes
N(2) C(10) 1.47(3) yes
N(3) O(3) 1.31(2) yes
C(2) C(3) 1.43(3) no
C(3) C(4) 1.39(2) no
C(4) C(5) 1.42(3) no
C(5) C(6) 1.34(2) no
C(6) C(2) 1.30(3) no
W' N(1)' 1.62(3) yes
W' O(2)' 2.130(10) yes
W' O(3)' 2.110(10) yes
W' C(1)' 2.19(2) yes
W' C(2)' 2.37(2) yes
W' C(3)' 2.34(2) yes
W' C(4)' 2.31(2) yes
W' C(5)' 2.38(2) yes
W' C(6)' 2.43(2) yes
W' Cp' 2.06 yes
Si(1)' C(1)' 1.86(2) yes
Si(1)' C(7)' 1.83(3) no
Si(1)' C(8)' 1.80(4) no
Si(1)' C(9)' 1.81(3) no
Si(2)' C(10)' 1.88(2) yes
Si(2)' C(11)' 1.68(3) no
Si(2)' C(12)' 1.83(2) no
Si(2)' C(13)' 1.94(3) no
N(1)' O(1)' 1.28(2) yes
N(2)' N(3)' 1.22(2) yes
N(2)' O(2)' 1.38(2) yes
N(2)' C(10)' 1.46(2) yes
N(3)' O(3)' 1.30(2) yes
C(2)' C(3)' 1.41(3) no
C(3)' C(4)' 1.40(3) no
C(4)' C(5)' 1.30(3) no
C(5)' C(6)' 1.37(3) no
C(6)' C(2)' 1.37(3) no
