#------------------------------------------------------------------------------
#$Date: 2017-10-14 21:27:35 +0200 (Sat 14 de Oct de 2017) $
#$Revision: 202017 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/38/7003887.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_7003887
loop_
_publ_author_name
'Clough, Christopher R.'
'Müller, Peter'
'Cummins, Christopher C.'
_publ_section_title
;
 6-Coordinate tungsten(vi) tris-n-isopropylanilide complexes: products
 of terminal oxo and nitrido transformations effected by main group
 electrophiles
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              4458
_journal_page_last               4463
_journal_paper_doi               10.1039/b801037d
_journal_year                    2008
_chemical_formula_sum            'C35 H48 Cl F3 N4 O W'
_chemical_formula_weight         817.07
_chemical_name_common            W(NC(O)CF3)(Cl)(N(i-Pr)Ar)3
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.0410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1298(6)
_cell_length_b                   10.4918(3)
_cell_length_c                   19.4084(5)
_cell_measurement_reflns_used    8634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.23
_cell_volume                     3529.67(18)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0907
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            73315
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    3.397
_exptl_absorpt_correction_T_max  0.9352
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0359
_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)+(0.0328P)²+1.4281P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                7001
_reflns_number_total             8736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801037d.txt
_cod_data_source_block           1-(NC(O)CF3)Cl
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003887
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.092820(9) 0.843115(14) 0.827802(8) 0.01431(5) Uani 1 1 d . . .
Cl1 Cl 0.22243(6) 0.73229(10) 0.86223(5) 0.0215(2) Uani 1 1 d . . .
F1 F 0.22661(17) 1.2110(3) 0.94102(16) 0.0419(7) Uani 1 1 d . . .
N1 N 0.05460(19) 0.7047(3) 0.87411(16) 0.0174(7) Uani 1 1 d . . .
O1 O 0.1605(3) 0.9985(5) 1.01097(18) 0.0765(16) Uani 1 1 d . . .
N2 N 0.09959(18) 0.8405(3) 0.72942(16) 0.0157(6) Uani 1 1 d . . .
F2 F 0.28647(14) 1.0530(3) 0.91204(13) 0.0336(6) Uani 1 1 d . . .
F3 F 0.29957(16) 1.0920(3) 1.02356(14) 0.0422(7) Uani 1 1 d . . .
N3 N -0.00352(19) 0.9418(3) 0.79865(17) 0.0173(7) Uani 1 1 d . . .
N4 N 0.14119(19) 0.9609(3) 0.89185(17) 0.0206(7) Uani 1 1 d . . .
C11 C -0.0236(2) 0.6580(4) 0.8504(2) 0.0195(8) Uani 1 1 d . . .
C12 C -0.0439(3) 0.5644(4) 0.7971(2) 0.0229(9) Uani 1 1 d . . .
H12 H -0.0064 0.5329 0.7760 0.028 Uiso 1 1 calc R . .
C13 C -0.1187(3) 0.5170(4) 0.7748(2) 0.0322(11) Uani 1 1 d . . .
C14 C -0.1728(3) 0.5635(4) 0.8061(2) 0.0324(11) Uani 1 1 d . . .
H14 H -0.2238 0.5305 0.7911 0.039 Uiso 1 1 calc R . .
C15 C -0.1544(3) 0.6566(4) 0.8586(2) 0.0298(10) Uani 1 1 d . . .
C16 C -0.0792(2) 0.7049(4) 0.8803(2) 0.0226(9) Uani 1 1 d . . .
H16 H -0.0660 0.7702 0.9158 0.027 Uiso 1 1 calc R . .
C17 C 0.1030(2) 0.6379(4) 0.9409(2) 0.0247(9) Uani 1 1 d . . .
H17 H 0.1554 0.6776 0.9539 0.030 Uiso 1 1 calc R . .
C18 C 0.1129(3) 0.4971(4) 0.9253(3) 0.0351(11) Uani 1 1 d . . .
H18A H 0.1331 0.4896 0.8838 0.053 Uiso 1 1 calc R . .
H18B H 0.0628 0.4540 0.9145 0.053 Uiso 1 1 calc R . .
H18C H 0.1490 0.4574 0.9675 0.053 Uiso 1 1 calc R . .
C19 C 0.0715(3) 0.6564(5) 1.0051(2) 0.0344(11) Uani 1 1 d . . .
H19A H 0.0661 0.7477 1.0131 0.052 Uiso 1 1 calc R . .
H19B H 0.1073 0.6184 1.0482 0.052 Uiso 1 1 calc R . .
H19C H 0.0211 0.6149 0.9952 0.052 Uiso 1 1 calc R . .
C21 C 0.0664(2) 0.7337(4) 0.6847(2) 0.0177(8) Uani 1 1 d . . .
C22 C 0.0925(2) 0.6102(4) 0.7056(2) 0.0207(9) Uani 1 1 d . . .
H22 H 0.1330 0.5974 0.7489 0.025 Uiso 1 1 calc R . .
C23 C 0.0596(3) 0.5055(4) 0.6633(2) 0.0226(9) Uani 1 1 d . . .
C24 C 0.0005(2) 0.5266(4) 0.5998(2) 0.0257(9) Uani 1 1 d . . .
H24 H -0.0228 0.4558 0.5711 0.031 Uiso 1 1 calc R . .
C25 C -0.0251(2) 0.6497(4) 0.5772(2) 0.0250(9) Uani 1 1 d . . .
C26 C 0.0087(2) 0.7520(4) 0.6206(2) 0.0207(9) Uani 1 1 d . . .
H26 H -0.0082 0.8362 0.6060 0.025 Uiso 1 1 calc R . .
C27 C 0.1352(2) 0.9366(4) 0.6923(2) 0.0208(9) Uani 1 1 d . . .
H27 H 0.0943 0.9685 0.6491 0.025 Uiso 1 1 calc R . .
C28 C 0.1981(3) 0.8733(4) 0.6667(2) 0.0281(10) Uani 1 1 d . . .
H28A H 0.1763 0.8004 0.6359 0.042 Uiso 1 1 calc R . .
H28B H 0.2396 0.8439 0.7084 0.042 Uiso 1 1 calc R . .
H28C H 0.2188 0.9349 0.6392 0.042 Uiso 1 1 calc R . .
C29 C 0.1680(3) 1.0504(4) 0.7404(2) 0.0238(9) Uani 1 1 d . . .
H29A H 0.1271 1.0903 0.7565 0.036 Uiso 1 1 calc R . .
H29B H 0.1887 1.1125 0.7131 0.036 Uiso 1 1 calc R . .
H29C H 0.2094 1.0216 0.7824 0.036 Uiso 1 1 calc R . .
C31 C -0.0562(2) 0.9456(4) 0.7258(2) 0.0180(8) Uani 1 1 d . . .
C32 C -0.0490(2) 1.0389(4) 0.6774(2) 0.0211(9) Uani 1 1 d . . .
H32 H -0.0095 1.1014 0.6919 0.025 Uiso 1 1 calc R . .
C33 C -0.0999(3) 1.0410(4) 0.6072(2) 0.0257(9) Uani 1 1 d . . .
C34 C -0.1572(2) 0.9498(4) 0.5879(2) 0.0271(10) Uani 1 1 d . . .
H34 H -0.1919 0.9510 0.5406 0.032 Uiso 1 1 calc R . .
C35 C -0.1657(2) 0.8559(4) 0.6360(2) 0.0250(9) Uani 1 1 d . . .
C36 C -0.1141(2) 0.8548(4) 0.7055(2) 0.0229(9) Uani 1 1 d . . .
H36 H -0.1188 0.7916 0.7390 0.027 Uiso 1 1 calc R . .
C37 C -0.0274(2) 1.0275(4) 0.8510(2) 0.0207(8) Uani 1 1 d . . .
H37 H -0.0033 0.9939 0.9007 0.025 Uiso 1 1 calc R . .
C38 C -0.1147(2) 1.0322(4) 0.8379(2) 0.0254(9) Uani 1 1 d . . .
H38A H -0.1342 0.9457 0.8403 0.038 Uiso 1 1 calc R . .
H38B H -0.1394 1.0685 0.7902 0.038 Uiso 1 1 calc R . .
H38C H -0.1264 1.0853 0.8748 0.038 Uiso 1 1 calc R . .
C39 C 0.0036(3) 1.1620(4) 0.8473(2) 0.0264(9) Uani 1 1 d . . .
H39A H 0.0595 1.1585 0.8557 0.040 Uiso 1 1 calc R . .
H39B H -0.0080 1.2154 0.8843 0.040 Uiso 1 1 calc R . .
H39C H -0.0210 1.1985 0.7996 0.040 Uiso 1 1 calc R . .
C41 C 0.1782(3) 1.0079(4) 0.9564(2) 0.0293(10) Uani 1 1 d . . .
C42 C 0.2485(3) 1.0908(4) 0.9576(2) 0.0294(10) Uani 1 1 d . . .
C131 C -0.1408(3) 0.4156(5) 0.7169(3) 0.0495(15) Uani 1 1 d . . .
H13A H -0.1524 0.3359 0.7379 0.074 Uiso 1 1 calc R . .
H13B H -0.0979 0.4018 0.6966 0.074 Uiso 1 1 calc R . .
H13C H -0.1864 0.4435 0.6787 0.074 Uiso 1 1 calc R . .
C151 C -0.2136(3) 0.7069(5) 0.8931(3) 0.0408(13) Uani 1 1 d . . .
H15A H -0.2656 0.6888 0.8616 0.061 Uiso 1 1 calc R . .
H15B H -0.2070 0.7991 0.9002 0.061 Uiso 1 1 calc R . .
H15C H -0.2064 0.6652 0.9398 0.061 Uiso 1 1 calc R . .
C231 C 0.0883(3) 0.3727(4) 0.6859(2) 0.0322(11) Uani 1 1 d . . .
H23A H 0.0499 0.3105 0.6600 0.048 Uiso 1 1 calc R . .
H23B H 0.0968 0.3629 0.7379 0.048 Uiso 1 1 calc R . .
H23C H 0.1369 0.3584 0.6746 0.048 Uiso 1 1 calc R . .
C251 C -0.0894(3) 0.6717(5) 0.5090(2) 0.0357(11) Uani 1 1 d . . .
H25A H -0.1382 0.6819 0.5205 0.054 Uiso 1 1 calc R . .
H25B H -0.0931 0.5986 0.4767 0.054 Uiso 1 1 calc R . .
H25C H -0.0787 0.7490 0.4852 0.054 Uiso 1 1 calc R . .
C331 C -0.0893(3) 1.1389(5) 0.5540(2) 0.0368(12) Uani 1 1 d . . .
H33A H -0.0441 1.1166 0.5385 0.055 Uiso 1 1 calc R . .
H33B H -0.0815 1.2231 0.5769 0.055 Uiso 1 1 calc R . .
H33C H -0.1352 1.1406 0.5120 0.055 Uiso 1 1 calc R . .
C351 C -0.2281(3) 0.7564(5) 0.6153(3) 0.0367(12) Uani 1 1 d . . .
H35A H -0.2514 0.7572 0.5629 0.055 Uiso 1 1 calc R . .
H35B H -0.2677 0.7751 0.6390 0.055 Uiso 1 1 calc R . .
H35C H -0.2058 0.6722 0.6305 0.055 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
N4 W1 N1 111.36(14) . . ?
N4 W1 N2 122.09(14) . . ?
N1 W1 N2 125.25(13) . . ?
N4 W1 N3 92.83(14) . . ?
N1 W1 N3 96.88(14) . . ?
N2 W1 N3 91.78(13) . . ?
N4 W1 Cl1 84.60(11) . . ?
N1 W1 Cl1 87.92(10) . . ?
N2 W1 Cl1 86.10(9) . . ?
N3 W1 Cl1 175.12(10) . . ?
C11 N1 C17 112.8(3) . . ?
C11 N1 W1 123.9(2) . . ?
C17 N1 W1 123.3(3) . . ?
C21 N2 C27 113.5(3) . . ?
C21 N2 W1 117.9(2) . . ?
C27 N2 W1 128.6(2) . . ?
C31 N3 C37 113.6(3) . . ?
C31 N3 W1 124.6(2) . . ?
C37 N3 W1 121.7(2) . . ?
C41 N4 W1 156.8(3) . . ?
C16 C11 C12 119.5(4) . . ?
C16 C11 N1 120.7(4) . . ?
C12 C11 N1 119.8(4) . . ?
C13 C12 C11 120.3(4) . . ?
C14 C13 C12 119.3(4) . . ?
C14 C13 C131 120.4(4) . . ?
C12 C13 C131 120.3(5) . . ?
C15 C14 C13 121.6(4) . . ?
C14 C15 C16 118.9(4) . . ?
C14 C15 C151 121.5(4) . . ?
C16 C15 C151 119.6(5) . . ?
C11 C16 C15 120.4(4) . . ?
N1 C17 C19 112.3(4) . . ?
N1 C17 C18 110.6(3) . . ?
C19 C17 C18 112.2(4) . . ?
C26 C21 C22 119.5(4) . . ?
C26 C21 N2 120.4(4) . . ?
C22 C21 N2 120.1(3) . . ?
C23 C22 C21 120.6(4) . . ?
C24 C23 C22 118.7(4) . . ?
C24 C23 C231 121.0(4) . . ?
C22 C23 C231 120.3(4) . . ?
C23 C24 C25 121.5(4) . . ?
C26 C25 C24 118.4(4) . . ?
C26 C25 C251 120.4(4) . . ?
C24 C25 C251 121.2(4) . . ?
C21 C26 C25 121.3(4) . . ?
N2 C27 C29 112.4(3) . . ?
N2 C27 C28 109.5(3) . . ?
C29 C27 C28 110.2(4) . . ?
C36 C31 C32 120.4(4) . . ?
C36 C31 N3 118.9(3) . . ?
C32 C31 N3 120.7(4) . . ?
C31 C32 C33 120.1(4) . . ?
C34 C33 C32 118.7(4) . . ?
C34 C33 C331 121.6(4) . . ?
C32 C33 C331 119.7(4) . . ?
C33 C34 C35 122.0(4) . . ?
C34 C35 C36 118.5(4) . . ?
C34 C35 C351 122.2(4) . . ?
C36 C35 C351 119.4(4) . . ?
C31 C36 C35 120.4(4) . . ?
N3 C37 C39 109.7(3) . . ?
N3 C37 C38 113.2(3) . . ?
C39 C37 C38 109.8(3) . . ?
O1 C41 N4 127.6(4) . . ?
O1 C41 C42 118.0(4) . . ?
N4 C41 C42 114.3(4) . . ?
F2 C42 F1 107.3(4) . . ?
F2 C42 F3 106.8(4) . . ?
F1 C42 F3 107.2(4) . . ?
F2 C42 C41 114.1(4) . . ?
F1 C42 C41 110.2(4) . . ?
F3 C42 C41 110.9(4) . . ?
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 N4 1.790(3) . ?
W1 N1 1.940(3) . ?
W1 N2 1.949(3) . ?
W1 N3 1.965(3) . ?
W1 Cl1 2.5298(10) . ?
F1 C42 1.333(5) . ?
N1 C11 1.442(5) . ?
N1 C17 1.508(5) . ?
O1 C41 1.199(5) . ?
N2 C21 1.437(5) . ?
N2 C27 1.491(5) . ?
F2 C42 1.331(5) . ?
F3 C42 1.342(5) . ?
N3 C31 1.457(5) . ?
N3 C37 1.512(5) . ?
N4 C41 1.330(5) . ?
C11 C16 1.393(6) . ?
C11 C12 1.394(6) . ?
C12 C13 1.388(6) . ?
C13 C14 1.385(7) . ?
C13 C131 1.514(6) . ?
C14 C15 1.380(7) . ?
C15 C16 1.398(6) . ?
C15 C151 1.516(7) . ?
C17 C19 1.527(6) . ?
C17 C18 1.529(6) . ?
C21 C26 1.385(5) . ?
C21 C22 1.399(5) . ?
C22 C23 1.396(5) . ?
C23 C24 1.394(6) . ?
C23 C231 1.507(6) . ?
C24 C25 1.399(6) . ?
C25 C26 1.392(6) . ?
C25 C251 1.503(6) . ?
C27 C29 1.524(5) . ?
C27 C28 1.525(6) . ?
C31 C36 1.388(6) . ?
C31 C32 1.388(5) . ?
C32 C33 1.405(6) . ?
C33 C34 1.381(6) . ?
C33 C331 1.508(6) . ?
C34 C35 1.397(6) . ?
C35 C36 1.397(6) . ?
C35 C351 1.504(6) . ?
C37 C39 1.528(6) . ?
C37 C38 1.529(6) . ?
C41 C42 1.537(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652659
