The Polar [WO2F4]2- Anion in the Solid State
Kevin R. Heier; Alexander J. Norquist; P. Shiv Halasyamani; Angel Duarte; Charlotte L. Stern; Kenneth R. Poeppelmeier; Inorganic Chemistry 38 (1999) 762–767; doi:10.1021/ic980863h

data_4321788
_publ_contact_author_address
;
Dept. of Chemistry 
Northwestern University
Evanston, IL 60208-3113
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_publ_contact_author_name        ' Poeppelmeier, Kenneth R.'
_publ_section_title
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 The Polar [WO2F4]2- Anion in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              762
_journal_page_last               767
_journal_paper_doi               10.1021/ic980863h
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'hydro(solvo)thermal synthesis'
_chemical_formula_moiety         'C12 H14 Cu F4 N6 O3 W'
_chemical_formula_sum            'C12 H14 Cu F4 N6 O3 W'
_chemical_formula_weight         613.67
_space_group_IT_number           123
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      123
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   6.886(3)
_cell_length_b                   6.886(3)
_cell_length_c                   8.300(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      12.6
_cell_measurement_theta_min      9.7
_cell_volume                     393.6(3)
_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      153.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       \w-\q
_diffrn_orient_matrix_UB_11      -0.01452
_diffrn_orient_matrix_UB_12      -0.08455
_diffrn_orient_matrix_UB_13      0.09715
_diffrn_orient_matrix_UB_21      -0.01484
_diffrn_orient_matrix_UB_22      -0.11618
_diffrn_orient_matrix_UB_23      -0.07122
_diffrn_orient_matrix_UB_31      0.14378
_diffrn_orient_matrix_UB_32      -0.02057
_diffrn_orient_matrix_UB_33      0.00245
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.08692
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1866
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        -0.60
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.735
_exptl_absorpt_correction_T_max  0.352
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.589
_exptl_crystal_density_meas      2.55(2)
_exptl_crystal_density_method    'flotation pycometry'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             291.00
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.02
_refine_diff_density_min         -1.26
_refine_ls_extinction_coef       0.0000147(7)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   3.514
_refine_ls_goodness_of_fit_ref   3.510
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     39
_refine_ls_number_reflns         366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0410
_refine_ls_wR_factor_ref         0.0410
_reflns_number_gt                366
_reflns_number_total             445
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic980863h_2.cif
_cod_data_source_block           '_S96-Cu/W/pyz_#2'
_cod_original_cell_volume        393.6(2)
_cod_database_code               4321788
_cod_depositor_comments
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Moving '_atom_site_refinement_flags' tag from the 7th loop position to 
the 9th loop position in 'atom_site' loop in accordance to data.

Antanas Vaitkus,
2015-03-25
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