#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:27:59 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178652 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/63/4076393.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_4076393
loop_
_publ_author_name
'van der Eide, Edwin F.'
'Liu, Tianbiao'
'Camaioni, Donald M.'
'Walter, Eric D.'
'Bullock, R. Morris'
_publ_section_title
;
 Facile Thermal W--W Bond Homolysis in the N-Heterocyclic Carbene
 Containing Tungsten Dimer [CpW(CO)2(IMe)]2
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1775
_journal_paper_doi               10.1021/om201162g
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C14 H16 N3 O2 W 1+, F6 P 1-'
_chemical_formula_sum            'C14 H16 F6 N3 O2 P W'
_chemical_formula_weight         587.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.5960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5707(3)
_cell_length_b                   12.0465(3)
_cell_length_c                   14.5973(4)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.61
_cell_volume                     1798.83(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0102
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30526
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    6.585
_exptl_absorpt_correction_T_max  0.6209
_exptl_absorpt_correction_T_min  0.5054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.480
_refine_diff_density_min         -2.058
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.698
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.698
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0146
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                4233
_reflns_number_total             4441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201162g_si_002.cif
_cod_data_source_block           edw7b_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4076393
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
W1 W 0.215337(7) 0.743887(7) 0.092982(5) 0.01152(6) Uani 1 1 d .
F3 F 0.80076(13) 0.54926(11) 0.09927(9) 0.0323(3) Uani 1 1 d .
F2 F 0.83766(18) 0.73014(13) 0.13413(14) 0.0295(3) Uani 1 1 d .
F5 F 0.58267(12) 0.57997(12) 0.06403(9) 0.0333(3) Uani 1 1 d .
F1 F 0.70884(12) 0.67985(11) -0.00838(8) 0.0261(3) Uani 1 1 d .
F4 F 0.71008(12) 0.63042(12) 0.20786(8) 0.0286(3) Uani 1 1 d .
F6 F 0.6199(2) 0.76163(11) 0.09976(16) 0.0293(4) Uani 1 1 d .
O1 O -0.04373(15) 0.78500(18) -0.06006(11) 0.0268(3) Uani 1 1 d .
N3 N 0.44848(13) 0.92182(13) 0.17695(10) 0.0137(3) Uani 1 1 d .
O2 O 0.05783(14) 0.92112(13) 0.17518(11) 0.0266(3) Uani 1 1 d .
C3 C 0.35764(18) 0.62153(16) 0.20047(13) 0.0198(4) Uani 1 1 d .
H3 H 0.4471 0.6380 0.2276 0.024 Uiso 1 1 calc R
C1 C 0.1339(2) 0.61255(18) 0.17419(14) 0.0207(4) Uani 1 1 d .
H1 H 0.0475 0.6218 0.1811 0.025 Uiso 1 1 calc R
C14 C 0.50268(18) 0.86103(17) 0.26462(12) 0.0199(4) Uani 1 1 d .
H14A H 0.4316 0.8255 0.2858 0.030 Uiso 1 1 calc R
H14B H 0.5494 0.9126 0.3134 0.030 Uiso 1 1 calc R
H14C H 0.5634 0.8042 0.2534 0.030 Uiso 1 1 calc R
P1 P 0.70949(4) 0.65528(5) 0.09915(3) 0.01722(13) Uani 1 1 d .
C8 C 0.34876(17) 0.70071(16) -0.08433(12) 0.0155(3) Uani 1 1 d .
C6 C 0.0538(2) 0.76989(18) -0.00491(17) 0.0165(4) Uani 1 1 d .
N2 N 0.32739(14) 0.97764(13) 0.04446(10) 0.0153(3) Uani 1 1 d .
C10 C 0.34142(17) 0.89306(17) 0.10770(13) 0.0136(3) Uani 1 1 d .
C9 C 0.41016(19) 0.66557(18) -0.15773(13) 0.0213(4) Uani 1 1 d .
H9A H 0.5044 0.6798 -0.1373 0.032 Uiso 1 1 calc R
H9B H 0.3726 0.7071 -0.2160 0.032 Uiso 1 1 calc R
H9C H 0.3951 0.5860 -0.1696 0.032 Uiso 1 1 calc R
C11 C 0.50196(17) 1.02039(15) 0.15557(12) 0.0171(4) Uani 1 1 d .
H11 H 0.5780 1.0561 0.1924 0.021 Uiso 1 1 calc R
C7 C 0.11880(19) 0.85681(17) 0.14642(13) 0.0173(4) Uani 1 1 d .
C12 C 0.42581(18) 1.05580(16) 0.07275(13) 0.0196(4) Uani 1 1 d .
H12 H 0.4371 1.1216 0.0399 0.024 Uiso 1 1 calc R
C5 C 0.16965(19) 0.55478(17) 0.10018(14) 0.0203(4) Uani 1 1 d .
H5 H 0.1118 0.5188 0.0483 0.024 Uiso 1 1 calc R
C2 C 0.25019(19) 0.65457(17) 0.23664(13) 0.0207(4) Uani 1 1 d .
H2 H 0.2551 0.6969 0.2923 0.025 Uiso 1 1 calc R
C13 C 0.22124(18) 0.99307(18) -0.04105(13) 0.0229(4) Uani 1 1 d .
H13A H 0.2331 0.9418 -0.0903 0.034 Uiso 1 1 calc R
H13B H 0.2223 1.0696 -0.0635 0.034 Uiso 1 1 calc R
H13C H 0.1373 0.9781 -0.0265 0.034 Uiso 1 1 calc R
C4 C 0.30745(19) 0.56029(17) 0.11757(14) 0.0200(4) Uani 1 1 d .
H4 H 0.3579 0.5277 0.0792 0.024 Uiso 1 1 calc R
N1 N 0.30114(19) 0.72616(15) -0.02555(14) 0.0168(3) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C6 W1 C7 74.66(9)
C6 W1 N1 84.03(9)
C7 W1 N1 138.46(8)
C6 W1 C10 109.51(8)
C7 W1 C10 76.18(7)
N1 W1 C10 78.10(7)
C6 W1 C1 96.71(9)
C7 W1 C1 88.40(9)
N1 W1 C1 129.84(7)
C10 W1 C1 144.29(7)
C6 W1 C2 130.55(9)
C7 W1 C2 86.69(8)
N1 W1 C2 132.93(7)
C10 W1 C2 109.67(7)
C1 W1 C2 36.31(7)
C6 W1 C5 92.11(8)
C7 W1 C5 121.36(8)
N1 W1 C5 94.19(7)
C10 W1 C5 155.87(7)
C1 W1 C5 35.70(7)
C2 W1 C5 59.39(7)
C6 W1 C3 150.21(8)
C7 W1 C3 117.90(7)
N1 W1 C3 98.24(7)
C10 W1 C3 99.96(7)
C1 W1 C3 59.10(7)
C2 W1 C3 35.29(7)
C5 W1 C3 58.13(7)
C6 W1 C4 120.13(8)
C7 W1 C4 143.50(8)
N1 W1 C4 78.03(7)
C10 W1 C4 121.34(6)
C1 W1 C4 58.30(7)
C2 W1 C4 57.92(7)
C5 W1 C4 34.69(7)
C3 W1 C4 34.00(7)
C10 N3 C11 111.21(16)
C10 N3 C14 126.40(16)
C11 N3 C14 122.37(15)
C4 C3 C2 107.65(17)
C4 C3 W1 73.69(11)
C2 C3 W1 69.03(10)
C4 C3 H3 126.2
C2 C3 H3 126.2
W1 C3 H3 122.8
C5 C1 C2 108.05(18)
C5 C1 W1 74.62(11)
C2 C1 W1 72.99(11)
C5 C1 H1 126.0
C2 C1 H1 126.0
W1 C1 H1 118.3
N3 C14 H14A 109.5
N3 C14 H14B 109.5
H14A C14 H14B 109.5
N3 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
F5 P1 F6 90.36(10)
F5 P1 F1 89.68(7)
F6 P1 F1 90.07(9)
F5 P1 F2 179.50(10)
F6 P1 F2 90.11(11)
F1 P1 F2 90.16(9)
F5 P1 F3 90.23(8)
F6 P1 F3 179.38(11)
F1 P1 F3 90.13(7)
F2 P1 F3 89.30(8)
F5 P1 F4 90.30(7)
F6 P1 F4 89.92(9)
F1 P1 F4 179.97(10)
F2 P1 F4 89.87(9)
F3 P1 F4 89.88(7)
N1 C8 C9 178.5(2)
O1 C6 W1 177.5(2)
C10 N2 C12 111.22(15)
C10 N2 C13 127.12(15)
C12 N2 C13 121.58(16)
N2 C10 N3 104.02(16)
N2 C10 W1 125.66(12)
N3 C10 W1 130.31(14)
C8 C9 H9A 109.5
C8 C9 H9B 109.5
H9A C9 H9B 109.5
C8 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
C12 C11 N3 106.82(15)
C12 C11 H11 126.6
N3 C11 H11 126.6
O2 C7 W1 177.22(17)
C11 C12 N2 106.69(16)
C11 C12 H12 126.7
N2 C12 H12 126.7
C1 C5 C4 107.51(17)
C1 C5 W1 69.67(11)
C4 C5 W1 75.37(11)
C1 C5 H5 126.2
C4 C5 H5 126.2
W1 C5 H5 120.5
C3 C2 C1 107.66(18)
C3 C2 W1 75.67(10)
C1 C2 W1 70.69(10)
C3 C2 H2 126.2
C1 C2 H2 126.2
W1 C2 H2 119.3
N2 C13 H13A 109.5
N2 C13 H13B 109.5
H13A C13 H13B 109.5
N2 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
C3 C4 C5 109.13(18)
C3 C4 W1 72.31(12)
C5 C4 W1 69.94(11)
C3 C4 H4 125.4
C5 C4 H4 125.4
W1 C4 H4 123.9
C8 N1 W1 169.87(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C6 1.956(2)
W1 C7 1.975(2)
W1 N1 2.1570(19)
W1 C10 2.215(2)
W1 C1 2.272(2)
W1 C2 2.3025(18)
W1 C5 2.337(2)
W1 C3 2.3890(18)
W1 C4 2.407(2)
F3 P1 1.6003(14)
F2 P1 1.6002(17)
F5 P1 1.5927(13)
F1 P1 1.5957(12)
F4 P1 1.6134(12)
F6 P1 1.5948(16)
O1 C6 1.151(3)
N3 C10 1.359(2)
N3 C11 1.384(2)
N3 C14 1.460(2)
O2 C7 1.152(2)
C3 C4 1.402(3)
C3 C2 1.425(3)
C3 H3 0.9500
C1 C5 1.414(3)
C1 C2 1.426(3)
C1 H1 0.9500
C14 H14A 0.9800
C14 H14B 0.9800
C14 H14C 0.9800
C8 N1 1.141(3)
C8 C9 1.449(2)
N2 C10 1.358(2)
N2 C12 1.387(2)
N2 C13 1.465(2)
C9 H9A 0.9800
C9 H9B 0.9800
C9 H9C 0.9800
C11 C12 1.342(3)
C11 H11 0.9500
C12 H12 0.9500
C5 C4 1.416(3)
C5 H5 0.9500
C2 H2 0.9500
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
C4 H4 0.9500
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
C6 W1 C3 C4 38.5(2)
C7 W1 C3 C4 147.30(12)
N1 W1 C3 C4 -53.88(12)
C10 W1 C3 C4 -133.15(11)
C1 W1 C3 C4 78.02(13)
C2 W1 C3 C4 116.77(17)
C5 W1 C3 C4 35.94(12)
C6 W1 C3 C2 -78.3(2)
C7 W1 C3 C2 30.53(14)
N1 W1 C3 C2 -170.65(12)
C10 W1 C3 C2 110.08(12)
C1 W1 C3 C2 -38.75(12)
C5 W1 C3 C2 -80.83(12)
C4 W1 C3 C2 -116.77(17)
C6 W1 C1 C5 84.24(13)
C7 W1 C1 C5 158.59(12)
N1 W1 C1 C5 -3.58(16)
C10 W1 C1 C5 -138.04(13)
C2 W1 C1 C5 -114.84(18)
C3 W1 C1 C5 -77.20(13)
C4 W1 C1 C5 -37.19(11)
C6 W1 C1 C2 -160.92(13)
C7 W1 C1 C2 -86.57(13)
N1 W1 C1 C2 111.26(13)
C10 W1 C1 C2 -23.20(19)
C5 W1 C1 C2 114.84(18)
C3 W1 C1 C2 37.64(12)
C4 W1 C1 C2 77.65(13)
C7 W1 C6 O1 -45(5)
N1 W1 C6 O1 171(5)
C10 W1 C6 O1 -114(5)
C1 W1 C6 O1 41(5)
C2 W1 C6 O1 26(5)
C5 W1 C6 O1 77(5)
C3 W1 C6 O1 74(5)
C4 W1 C6 O1 98(5)
C12 N2 C10 N3 1.54(19)
C13 N2 C10 N3 -175.29(17)
C12 N2 C10 W1 -177.29(13)
C13 N2 C10 W1 5.9(3)
C11 N3 C10 N2 -1.83(19)
C14 N3 C10 N2 177.02(16)
C11 N3 C10 W1 176.92(13)
C14 N3 C10 W1 -4.2(3)
C6 W1 C10 N2 -15.71(18)
C7 W1 C10 N2 -83.61(16)
N1 W1 C10 N2 63.49(15)
C1 W1 C10 N2 -150.57(14)
C2 W1 C10 N2 -164.91(15)
C5 W1 C10 N2 136.75(17)
C3 W1 C10 N2 159.90(15)
C4 W1 C10 N2 131.37(15)
C6 W1 C10 N3 165.78(16)
C7 W1 C10 N3 97.88(17)
N1 W1 C10 N3 -115.03(17)
C1 W1 C10 N3 30.9(2)
C2 W1 C10 N3 16.57(18)
C5 W1 C10 N3 -41.8(3)
C3 W1 C10 N3 -18.61(17)
C4 W1 C10 N3 -47.15(18)
C10 N3 C11 C12 1.5(2)
C14 N3 C11 C12 -177.44(16)
C6 W1 C7 O2 25(4)
N1 W1 C7 O2 86(4)
C10 W1 C7 O2 140(4)
C1 W1 C7 O2 -73(4)
C2 W1 C7 O2 -109(4)
C5 W1 C7 O2 -58(4)
C3 W1 C7 O2 -126(4)
C4 W1 C7 O2 -96(4)
N3 C11 C12 N2 -0.5(2)
C10 N2 C12 C11 -0.7(2)
C13 N2 C12 C11 176.33(17)
C2 C1 C5 C4 0.6(2)
W1 C1 C5 C4 66.46(13)
C2 C1 C5 W1 -65.88(14)
C6 W1 C5 C1 -98.59(13)
C7 W1 C5 C1 -25.31(15)
N1 W1 C5 C1 177.25(12)
C10 W1 C5 C1 107.28(18)
C2 W1 C5 C1 38.64(12)
C3 W1 C5 C1 80.14(13)
C4 W1 C5 C1 115.36(16)
C6 W1 C5 C4 146.05(13)
C7 W1 C5 C4 -140.67(12)
N1 W1 C5 C4 61.88(12)
C10 W1 C5 C4 -8.1(2)
C1 W1 C5 C4 -115.36(16)
C2 W1 C5 C4 -76.73(12)
C3 W1 C5 C4 -35.22(11)
C4 C3 C2 C1 -0.1(2)
W1 C3 C2 C1 63.93(13)
C4 C3 C2 W1 -64.05(14)
C5 C1 C2 C3 -0.3(2)
W1 C1 C2 C3 -67.25(13)
C5 C1 C2 W1 66.96(14)
C6 W1 C2 C3 140.20(13)
C7 W1 C2 C3 -153.27(12)
N1 W1 C2 C3 12.69(16)
C10 W1 C2 C3 -79.22(12)
C1 W1 C2 C3 114.91(18)
C5 W1 C2 C3 76.93(12)
C4 W1 C2 C3 36.11(11)
C6 W1 C2 C1 25.29(17)
C7 W1 C2 C1 91.82(14)
N1 W1 C2 C1 -102.22(14)
C10 W1 C2 C1 165.87(12)
C5 W1 C2 C1 -37.98(12)
C3 W1 C2 C1 -114.91(18)
C4 W1 C2 C1 -78.80(13)
C2 C3 C4 C5 0.5(2)
W1 C3 C4 C5 -60.55(13)
C2 C3 C4 W1 61.03(13)
C1 C5 C4 C3 -0.7(2)
W1 C5 C4 C3 62.02(14)
C1 C5 C4 W1 -62.69(13)
C6 W1 C4 C3 -159.05(13)
C7 W1 C4 C3 -53.38(18)
N1 W1 C4 C3 125.19(13)
C10 W1 C4 C3 57.28(13)
C1 W1 C4 C3 -80.56(13)
C2 W1 C4 C3 -37.50(11)
C5 W1 C4 C3 -118.86(18)
C6 W1 C4 C5 -40.19(15)
C7 W1 C4 C5 65.48(17)
N1 W1 C4 C5 -115.95(12)
C10 W1 C4 C5 176.14(11)
C1 W1 C4 C5 38.30(12)
C2 W1 C4 C5 81.36(13)
C3 W1 C4 C5 118.86(18)
C9 C8 N1 W1 -11(9)
C6 W1 N1 C8 -111.9(10)
C7 W1 N1 C8 -170.6(9)
C10 W1 N1 C8 136.7(10)
C1 W1 N1 C8 -18.1(10)
C2 W1 N1 C8 30.8(10)
C5 W1 N1 C8 -20.2(10)
C3 W1 N1 C8 38.1(10)
C4 W1 N1 C8 10.6(9)
