#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:23:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180010 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/04/7030472.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_7030472
loop_
_publ_author_name
'Bonsu, Richard O.'
'Kim, Hankook'
'O'Donohue, Christopher'
'Korotkov, Roman Y.'
'McClain, K. Randall'
'Abboud, Khalil A.'
'Ellsworth, Ashley A.'
'Walker, Amy V.'
'Anderson, Timothy J.'
'McElwee-White, Lisa'
_publ_section_title
;
 Partially fluorinated oxo-alkoxide tungsten(vi) complexes as precursors
 for deposition of WOx nanomaterials.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9226
_journal_page_last               9233
_journal_paper_doi               10.1039/c4dt00407h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C16 H24 F12 O5 W'
_chemical_formula_weight         708.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-07-16 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.173(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1356(18)
_cell_length_b                   6.0103(6)
_cell_length_c                   20.6144(19)
_cell_measurement_reflns_used    6015
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      3.56
_cell_volume                     2310.3(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10645
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    5.121
_exptl_absorpt_correction_T_max  0.6848
_exptl_absorpt_correction_T_min  0.4946
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.774
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0163P)²+8.8188P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                2517
_reflns_number_total             2652
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c4dt00407h2.cif
_cod_data_source_block           bonsu8
_cod_depositor_comments
'Adding full bibliography for 7030471--7030472.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7030472
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.0000 0.26605(3) 0.2500 0.01076(5) Uani 1 2 d S
F1 F -0.02595(9) -0.0191(3) 0.41476(9) 0.0258(4) Uani 1 1 d .
F2 F -0.02829(9) 0.3103(3) 0.45531(9) 0.0242(4) Uani 1 1 d .
F3 F -0.11959(10) 0.0920(3) 0.43220(9) 0.0265(4) Uani 1 1 d .
F4 F 0.1904(1) 0.6888(4) 0.33967(10) 0.0329(5) Uani 1 1 d .
F5 F 0.23331(9) 0.3599(4) 0.36725(10) 0.0299(5) Uani 1 1 d .
F6 F 0.24085(9) 0.5963(3) 0.44792(9) 0.0264(4) Uani 1 1 d .
O1 O 0.0000 -0.0167(5) 0.2500 0.0208(6) Uani 1 2 d S
O2 O -0.04046(10) 0.3138(3) 0.3185(1) 0.0146(4) Uani 1 1 d .
O3 O 0.0867(1) 0.3713(4) 0.31592(10) 0.0216(5) Uani 1 1 d .
C1 C -0.10041(14) 0.2473(5) 0.33497(14) 0.0148(5) Uani 1 1 d .
C2 C -0.06790(15) 0.1571(5) 0.40976(14) 0.0158(6) Uani 1 1 d .
C3 C -0.14545(16) 0.4527(6) 0.33295(18) 0.0251(7) Uani 1 1 d .
H3A H -0.1158 0.5637 0.3661 0.038 Uiso 1 1 calc R
H3B H -0.1859 0.4112 0.3459 0.038 Uiso 1 1 calc R
H3C H -0.1636 0.5155 0.2856 0.038 Uiso 1 1 calc R
C4 C -0.14367(16) 0.0636(6) 0.28644(15) 0.0217(7) Uani 1 1 d .
H4A H -0.1650 0.1207 0.2384 0.033 Uiso 1 1 calc R
H4B H -0.1818 0.0139 0.3017 0.033 Uiso 1 1 calc R
H4C H -0.1120 -0.0619 0.2880 0.033 Uiso 1 1 calc R
C5 C 0.12565(14) 0.4434(5) 0.38593(14) 0.0142(5) Uani 1 1 d .
C6 C 0.19764(15) 0.5221(5) 0.38509(15) 0.0183(6) Uani 1 1 d .
C7 C 0.13844(17) 0.2516(5) 0.43638(17) 0.0261(7) Uani 1 1 d .
H7A H 0.1645 0.1335 0.4233 0.039 Uiso 1 1 calc R
H7B H 0.0923 0.1938 0.4347 0.039 Uiso 1 1 calc R
H7C H 0.1668 0.3029 0.4840 0.039 Uiso 1 1 calc R
C8 C 0.08768(16) 0.6383(5) 0.40370(16) 0.0211(6) Uani 1 1 d .
H8A H 0.0782 0.7533 0.3676 0.032 Uiso 1 1 calc R
H8B H 0.1181 0.6999 0.4493 0.032 Uiso 1 1 calc R
H8C H 0.0422 0.5875 0.4057 0.032 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'
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'
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
O1 W1 O3 109.74(7) . .
O1 W1 O3 109.74(7) . 2
O3 W1 O3 140.51(15) . 2
O1 W1 O2 98.70(6) . .
O3 W1 O2 87.33(8) . .
O3 W1 O2 86.82(8) 2 .
O1 W1 O2 98.70(6) . 2
O3 W1 O2 86.82(8) . 2
O3 W1 O2 87.33(8) 2 2
O2 W1 O2 162.60(13) . 2
C1 O2 W1 140.54(17) . .
C5 O3 W1 147.55(17) . .
O2 C1 C4 111.8(2) . .
O2 C1 C3 108.3(2) . .
C4 C1 C3 112.5(2) . .
O2 C1 C2 105.1(2) . .
C4 C1 C2 109.1(2) . .
C3 C1 C2 109.8(2) . .
F1 C2 F2 107.4(2) . .
F1 C2 F3 107.0(2) . .
F2 C2 F3 106.9(2) . .
F1 C2 C1 112.1(2) . .
F2 C2 C1 112.2(2) . .
F3 C2 C1 110.9(2) . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O3 C5 C7 110.6(2) . .
O3 C5 C8 110.1(2) . .
C7 C5 C8 113.2(2) . .
O3 C5 C6 104.1(2) . .
C7 C5 C6 109.2(2) . .
C8 C5 C6 109.2(2) . .
F6 C6 F4 106.7(2) . .
F6 C6 F5 106.7(2) . .
F4 C6 F5 106.2(2) . .
F6 C6 C5 111.4(2) . .
F4 C6 C5 112.6(2) . .
F5 C6 C5 112.7(3) . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.700(3) .
W1 O3 1.8718(19) .
W1 O3 1.8718(19) 2
W1 O2 1.8995(18) .
W1 O2 1.8995(18) 2
F1 C2 1.335(3) .
F2 C2 1.342(3) .
F3 C2 1.347(3) .
F4 C6 1.341(4) .
F5 C6 1.342(3) .
F6 C6 1.335(3) .
O2 C1 1.429(3) .
O3 C5 1.425(3) .
C1 C4 1.523(4) .
C1 C3 1.523(4) .
C1 C2 1.529(4) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C7 1.508(4) .
C5 C8 1.517(4) .
C5 C6 1.531(4) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
