#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/04/4320447.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_4320447
loop_
_publ_author_name
'Margaret E. Welk'
'Alexander J. Norquist'
'Charlotte L. Stern'
'Kenneth R. Poeppelmeier'
_publ_section_title
;
 The Ordered [WO2F4]2- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5479
_journal_page_last               5480
_journal_paper_doi               10.1021/ic015554x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C32 H36 Cu F8 N6 O6 W2'
_chemical_formula_weight         1183.91
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00(1)
_cell_angle_beta                 92.57(2)
_cell_angle_gamma                90.00(1)
_cell_formula_units_Z            4
_cell_length_a                   10.900(3)
_cell_length_b                   16.099(2)
_cell_length_c                   21.424(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     3755.7(13)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution
;
SHELX97 (Sheldrick, 1997)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku CCD'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03310
_diffrn_reflns_av_sigmaI/netI    0.036
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17352
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         0.95
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    67.70
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2268.00
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.63
_refine_diff_density_min         -1.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.328
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     324
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          2.0900
_refine_ls_shift/su_mean         0.0072
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0200
_refine_ls_wR_factor_ref         0.0200
_reflns_number_gt                3735
_reflns_number_total             4655
_reflns_threshold_expression     I>3.00σ(I)
_cod_data_source_file            ic015554x_s.cif
_cod_data_source_block           '_s11j.cif'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3756(1)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C32 H36 Cu F8 N6 O6 W2 '
_cod_database_code               4320447
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'   -x,   +y,1/2-z'
'   -x,   -y,   -z'
'   +x,   -y,1/2+z'
'1/2+x,1/2+y,   +z'
1/2-x,1/2+y,1/2-z
'1/2-x,1/2-y,   -z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
W(1) 0.75709(1) 0.072612(7) 0.389840(5) 0.01971(3) 1.000 . Uani d ?
Cu(2) 1.0000 0.06448(3) 0.2500 0.0156(1) 0.500 S Uani d ?
F(1) 0.6670(2) -0.0310(1) 0.35497(8) 0.0278(5) 1.000 . Uani d ?
F(2) 0.6362(1) 0.1282(1) 0.33793(7) 0.0249(4) 1.000 . Uani d ?
F(3) 0.8400(2) -0.0067(1) 0.44235(8) 0.0342(5) 1.000 . Uani d ?
F(4) 0.6199(2) 0.0616(1) 0.45025(8) 0.0292(5) 1.000 . Uani d ?
O(1) 0.8620(2) 0.0636(1) 0.32941(8) 0.0178(5) 1.000 . Uani d ?
O(2) 0.8117(2) 0.1602(1) 0.42712(9) 0.0308(6) 1.000 . Uani d ?
O(3) 0.7239(2) -0.1801(2) 0.3801(1) 0.0337(7) 1.000 . Uani d ?
N(1) 1.0000 -0.0630(2) 0.2500 0.0182(8) 0.500 S Uani d ?
N(2) 0.8580(2) 0.0579(1) 0.1851(1) 0.0171(6) 1.000 . Uani d ?
N(3) 1.0000 0.1917(2) 0.2500 0.0194(8) 0.500 S Uani d ?
N(4) 0.5107(2) -0.1848(2) 0.5042(1) 0.0223(6) 1.000 . Uani d ?
C(1) 0.8988(3) -0.1064(2) 0.2624(1) 0.0222(8) 1.000 . Uani d ?
C(2) 0.8953(3) -0.1920(2) 0.2625(1) 0.0262(8) 1.000 . Uani d ?
C(3) 1.0000 -0.2347(3) 0.2500 0.028(1) 0.500 S Uani d ?
C(4) 0.8722(3) 0.0170(2) 0.1309(1) 0.0201(7) 1.000 . Uani d ?
C(5) 0.7745(3) -0.0009(2) 0.0896(1) 0.0236(8) 1.000 . Uani d ?
C(6) 0.6585(3) 0.0234(2) 0.1042(1) 0.0287(8) 1.000 . Uani d ?
C(7) 0.6429(3) 0.0661(2) 0.1591(1) 0.0279(8) 1.000 . Uani d ?
C(8) 0.7443(3) 0.0827(2) 0.1980(1) 0.0219(7) 1.000 . Uani d ?
C(9) 1.0416(3) 0.2354(2) 0.2016(1) 0.0264(8) 1.000 . Uani d ?
C(10) 1.0445(3) 0.3212(2) 0.2007(2) 0.0347(9) 1.000 . Uani d ?
C(11) 1.0000 0.3653(3) 0.2500 0.038(1) 0.500 S Uani d ?
C(12) 0.5100(3) -0.2647(2) 0.5207(1) 0.0233(8) 1.000 . Uani d ?
C(13) 0.5839(3) -0.3184(2) 0.4883(1) 0.0252(8) 1.000 . Uani d ?
C(14) 0.6539(3) -0.2892(2) 0.4416(1) 0.0245(8) 1.000 . Uani d ?
C(15) 0.6525(3) -0.2053(2) 0.4257(1) 0.0240(8) 1.000 . Uani d ?
C(16) 0.5796(3) -0.1532(2) 0.4586(1) 0.0234(8) 1.000 . Uani d ?
C(17) 0.4300(4) -0.2912(2) 0.5719(2) 0.034(1) 1.000 . Uani d ?
H(1) 0.836(2) -0.079(2) 0.269(1) 0.014(7) 1.000 . Uiso d ?
H(2) 0.822(3) -0.216(2) 0.271(1) 0.030(8) 1.000 . Uiso d ?
H(3) 1.0000 -0.288(3) 0.2500 0.04(1) 0.500 S Uiso d ?
H(4) 0.951(2) -0.001(2) 0.124(1) 0.019(7) 1.000 . Uiso d ?
H(5) 0.790(3) -0.029(2) 0.053(1) 0.023(8) 1.000 . Uiso d ?
H(6) 0.591(3) 0.012(2) 0.078(1) 0.023(8) 1.000 . Uiso d ?
H(7) 0.569(3) 0.084(2) 0.169(1) 0.030(8) 1.000 . Uiso d ?
H(8) 0.741(3) 0.109(2) 0.233(1) 0.035(9) 1.000 . Uiso d ?
H(9) 1.072(3) 0.203(2) 0.168(1) 0.030(8) 1.000 . Uiso d ?
H(10) 1.077(3) 0.351(2) 0.165(2) 0.05(1) 1.000 . Uiso d ?
H(11) 1.0000 0.419(3) 0.2500 0.04(1) 0.500 S Uiso d ?
H(12) 0.591(3) -0.370(2) 0.498(1) 0.028(8) 1.000 . Uiso d ?
H(13) 0.703(3) -0.323(2) 0.422(1) 0.025(8) 1.000 . Uiso d ?
H(14) 0.712(4) -0.139(2) 0.372(2) 0.04(1) 1.000 . Uiso d ?
H(15) 0.572(3) -0.104(2) 0.451(1) 0.024(8) 1.000 . Uiso d ?
H(16) 0.464(3) -0.150(2) 0.524(1) 0.019(8) 1.000 . Uiso d ?
H(17) 0.423(3) -0.247(2) 0.603(2) 0.05(1) 1.000 . Uiso d ?
H(18) 0.465(3) -0.338(3) 0.593(2) 0.06(1) 1.000 . Uiso d ?
H(19) 0.354(3) -0.301(2) 0.558(2) 0.06(1) 1.000 . Uiso d ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 128 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
H 0 144 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N 0 24 0.004 0.003
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 24 0.008 0.006
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
F 0 32 0.014 0.010
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Cu 0 4 0.263 1.266
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
W 0 8 -1.421 6.872
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
