#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/40/4324050.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_4324050
loop_
_publ_author_name
'Katrin Köhler'
'Herbert W. Roesky'
'Axel Herzog'
'Heinz Gornitzka'
'Alexander Steiner'
'Isabel Usón'
_publ_section_title
;
 Syntheses, Structures, and Reactivity of a Series of
 (Pentamethylcyclopentadienyl)molybdenum(V) and -tungsten(V) Imido
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1773
_journal_page_last               1777
_journal_paper_doi               10.1021/ic950919x
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C16 H17 F5 N O2.5 W'
_chemical_formula_weight         542.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 104.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.246(3)
_cell_length_b                   10.043(2)
_cell_length_c                   14.102(3)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     1817.3(7)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    'Siemens SHELXTL-Plus'
_computing_publication_material  'SHELXTL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device
'Stoe-Siemens-AED2 four-circle-diffractometer'
_diffrn_measurement_method       'Profile data from 2theta/omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3977
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         4.06
_diffrn_standards_decay_%        15
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.417
_exptl_absorpt_correction_T_max  0.9690
_exptl_absorpt_correction_T_min  0.4015
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.037
_refine_diff_density_min         -1.227
_refine_diff_density_rms         .119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2345
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.019
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_obs          0.0295
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s²(Fo²)+( 0.0469P)²+4.0294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0765
_refine_ls_wR_factor_obs         0.0735
_reflns_number_observed          2221
_reflns_number_total             2349
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950919x_1.cif
_cod_data_source_block           hallo2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0469P)^2^+4.0294P] 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^)+( 0.0469P)^2^+4.0294P] 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        1817.3(6)
_cod_original_formula_sum        'C16 H17 F5 N O2.50 W'
_cod_database_code               4324050
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W1 W -0.13177(2) -0.03365(2) 0.41586(2) 0.02853(14) Uani 1 d U .
O1 O 0.0000 0.0000 0.5000 0.0390(14) Uani 1 d SU .
O2 O -0.1901(3) 0.1204(4) 0.3952(3) 0.0490(11) Uani 1 d U .
O3 O -0.1069(4) -0.0756(5) 0.3055(3) 0.0512(11) Uani 1 d U .
C1 C -0.2671(5) -0.0891(6) 0.4947(5) 0.0411(13) Uani 1 d U .
C2 C -0.2805(5) -0.1607(7) 0.4052(5) 0.0461(14) Uani 1 d U .
C3 C -0.1979(5) -0.2571(6) 0.4171(4) 0.0385(13) Uani 1 d U .
C4 C -0.1333(4) -0.2388(5) 0.5116(4) 0.0305(12) Uani 1 d U .
C5 C -0.1765(4) -0.1353(6) 0.5591(4) 0.0325(12) Uani 1 d U .
C11 C -0.3388(6) 0.0179(8) 0.5149(8) 0.070(2) Uani 1 d U .
H11A H -0.3985(26) -0.0235(8) 0.5328(47) 0.105 Uiso 1 calc R .
H11B H -0.3636(39) 0.0725(40) 0.4561(16) 0.105 Uiso 1 calc R .
H11C H -0.3011(16) 0.0742(39) 0.5689(31) 0.105 Uiso 1 calc R .
C12 C -0.3701(6) -0.1488(9) 0.3149(6) 0.077(3) Uani 1 d U .
H12A H -0.3990(33) -0.0585(23) 0.3111(26) 0.116 Uiso 1 calc R .
H12B H -0.4244(24) -0.2133(47) 0.3189(24) 0.116 Uiso 1 calc R .
H12C H -0.3450(13) -0.1668(64) 0.2564(7) 0.116 Uiso 1 calc R .
C13 C -0.1819(7) -0.3568(7) 0.3436(5) 0.069(2) Uani 1 d U .
H13A H -0.2362(28) -0.3459(40) 0.2827(16) 0.103 Uiso 1 calc R .
H13B H -0.1856(47) -0.4468(7) 0.3693(19) 0.103 Uiso 1 calc R .
H13C H -0.1133(20) -0.3430(39) 0.3307(33) 0.103 Uiso 1 calc R .
C14 C -0.0343(5) -0.3138(6) 0.5558(5) 0.044(2) Uani 1 d U .
H14A H -0.0027(18) -0.3440(37) 0.5037(6) 0.066 Uiso 1 calc R .
H14B H -0.0502(7) -0.3911(25) 0.5920(26) 0.066 Uiso 1 calc R .
H14C H 0.0145(14) -0.2552(14) 0.6006(24) 0.066 Uiso 1 calc R .
C15 C -0.1300(5) -0.0849(7) 0.6611(4) 0.048(2) Uani 1 d U .
H15A H -0.0539(6) -0.0836(45) 0.6735(13) 0.072 Uiso 1 calc R .
H15B H -0.1505(30) -0.1437(27) 0.7086(5) 0.072 Uiso 1 calc R .
H15C H -0.1554(29) 0.0055(19) 0.6677(11) 0.072 Uiso 1 calc R .
N1 N -0.1809(5) -0.1469(6) 0.0966(4) 0.059(2) Uani 1 d U .
C22 C -0.1825(7) -0.0594(7) 0.0223(6) 0.056(2) Uani 1 d U .
C23 C -0.1084(7) 0.0470(7) 0.0332(7) 0.062(2) Uani 1 d U .
F1 F -0.0395(4) 0.0582(4) 0.1175(4) 0.0779(14) Uani 1 d U .
C24 C -0.1107(9) 0.1340(8) -0.0426(8) 0.081(2) Uani 1 d U .
F2 F -0.0377(5) 0.2304(5) -0.0285(5) 0.115(2) Uani 1 d U .
C25 C -0.1824(10) 0.1224(10) -0.1296(8) 0.088(2) Uani 1 d U .
F3 F -0.1846(7) 0.2065(6) -0.2051(5) 0.142(3) Uani 1 d U .
C26 C -0.2560(9) 0.0237(10) -0.1418(7) 0.082(2) Uani 1 d U .
F4 F -0.3299(6) 0.0113(7) -0.2256(4) 0.117(2) Uani 1 d U .
C27 C -0.2544(7) -0.0674(9) -0.0684(6) 0.065(2) Uani 1 d U .
F5 F -0.3287(4) -0.1645(6) -0.0812(3) 0.0805(13) Uani 1 d U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 '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
O2 W1 O3 104.2(2) . . ?
O2 W1 O1 104.62(14) . . ?
O3 W1 O1 105.0(2) . . ?
O2 W1 C2 98.3(2) . . ?
O3 W1 C2 99.0(2) . . ?
O1 W1 C2 141.21(15) . . ?
O2 W1 C1 86.1(2) . . ?
O3 W1 C1 134.1(2) . . ?
O1 W1 C1 115.6(2) . . ?
C2 W1 C1 35.1(2) . . ?
O2 W1 C3 133.5(2) . . ?
O3 W1 C3 86.0(2) . . ?
O1 W1 C3 116.40(14) . . ?
C2 W1 C3 35.3(2) . . ?
C1 W1 C3 57.7(2) . . ?
O2 W1 C5 108.8(2) . . ?
O3 W1 C5 141.2(2) . . ?
O1 W1 C5 86.06(13) . . ?
C2 W1 C5 56.8(2) . . ?
C1 W1 C5 33.3(2) . . ?
C3 W1 C5 56.4(2) . . ?
O2 W1 C4 141.2(2) . . ?
O3 W1 C4 108.6(2) . . ?
O1 W1 C4 86.40(12) . . ?
C2 W1 C4 56.9(2) . . ?
C1 W1 C4 56.2(2) . . ?
C3 W1 C4 33.5(2) . . ?
C5 W1 C4 33.8(2) . . ?
W1 O1 W1 180.0 . 3_556 ?
C5 C1 C2 107.9(6) . . ?
C5 C1 C11 126.6(7) . . ?
C2 C1 C11 125.5(6) . . ?
C5 C1 W1 76.0(3) . . ?
C2 C1 W1 69.5(3) . . ?
C11 C1 W1 120.1(5) . . ?
C1 C2 C3 108.2(5) . . ?
C1 C2 C12 127.1(7) . . ?
C3 C2 C12 124.5(7) . . ?
C1 C2 W1 75.4(3) . . ?
C3 C2 W1 75.8(3) . . ?
C12 C2 W1 119.2(4) . . ?
C4 C3 C2 106.8(5) . . ?
C4 C3 C13 125.9(6) . . ?
C2 C3 C13 127.2(6) . . ?
C4 C3 W1 75.4(3) . . ?
C2 C3 W1 68.9(3) . . ?
C13 C3 W1 120.3(4) . . ?
C3 C4 C5 108.6(5) . . ?
C3 C4 C14 126.2(5) . . ?
C5 C4 C14 125.3(5) . . ?
C3 C4 W1 71.1(3) . . ?
C5 C4 W1 73.0(3) . . ?
C14 C4 W1 121.3(4) . . ?
C1 C5 C4 108.5(5) . . ?
C1 C5 C15 126.4(6) . . ?
C4 C5 C15 125.2(5) . . ?
C1 C5 W1 70.8(3) . . ?
C4 C5 W1 73.2(3) . . ?
C15 C5 W1 121.3(4) . . ?
N1 C22 C27 123.0(8) . . ?
N1 C22 C23 121.2(8) . . ?
C27 C22 C23 115.7(8) . . ?
F1 C23 C24 121.7(9) . . ?
F1 C23 C22 117.7(7) . . ?
C24 C23 C22 120.6(9) . . ?
F2 C24 C25 120.8(9) . . ?
F2 C24 C23 117.7(10) . . ?
C25 C24 C23 121.5(10) . . ?
F3 C25 C24 122.1(11) . . ?
F3 C25 C26 118.4(11) . . ?
C24 C25 C26 119.5(8) . . ?
F4 C26 C25 121.3(10) . . ?
F4 C26 C27 118.2(11) . . ?
C25 C26 C27 120.5(10) . . ?
F5 C27 C26 119.9(9) . . ?
F5 C27 C22 117.9(7) . . ?
C26 C27 C22 122.1(10) . . ?
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 O2 1.722(4) . ?
W1 O3 1.721(5) . ?
W1 O1 1.8817(7) . ?
W1 C2 2.320(6) . ?
W1 C1 2.397(6) . ?
W1 C3 2.411(6) . ?
W1 C5 2.463(6) . ?
W1 C4 2.466(5) . ?
O1 W1 1.8817(7) 3_556 ?
C1 C5 1.392(8) . ?
C1 C2 1.426(10) . ?
C1 C11 1.508(10) . ?
C2 C3 1.438(9) . ?
C2 C12 1.515(8) . ?
C3 C4 1.406(8) . ?
C3 C13 1.493(9) . ?
C4 C5 1.431(8) . ?
C4 C14 1.507(8) . ?
C5 C15 1.505(8) . ?
N1 C22 1.363(9) . ?
C22 C27 1.394(12) . ?
C22 C23 1.433(11) . ?
C23 F1 1.312(10) . ?
C23 C24 1.376(12) . ?
C24 F2 1.347(11) . ?
C24 C25 1.36(2) . ?
C25 F3 1.354(10) . ?
C25 C26 1.371(15) . ?
C26 F4 1.340(12) . ?
C26 C27 1.378(13) . ?
C27 F5 1.366(10) . ?
