Syntheses of two vanadium oxide-fluoride materials that differ in phase matchability.
Donakowski, Martin D.; Gautier, Romain; Lu, Hongcheng; Tran, T. Thao; Cantwell, Jacqueline R.; Halasyamani, P. Shiv; Poeppelmeier, Kenneth R.; Inorganic chemistry 54 (2015) 765–772; doi:10.1021/ic501486x

data_4340864
_publ_section_title
;
 Syntheses of two vanadium oxide-fluoride materials that differ in phase
 matchability.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              765
_journal_page_last               772
_journal_paper_doi               10.1021/ic501486x
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'F2 V, 2.67(F), 3.33(O), V, 2(Na)'
_chemical_formula_sum            'F4.67 Na2 O3.33 V2'
_chemical_formula_weight         289.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             2014-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.787(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3742(3)
_cell_length_b                   3.5963(2)
_cell_length_c                   14.3641(7)
_cell_measurement_reflns_used    3201
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.212
_cell_measurement_theta_min      3.418
_cell_volume                     307.84(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.05
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10434
_diffrn_reflns_point_group_measured_fraction_full 0.701
_diffrn_reflns_point_group_measured_fraction_max 0.623
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         43.097
_diffrn_reflns_theta_min         3.210
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.236
_exptl_absorpt_correction_T_max  0.7429
_exptl_absorpt_correction_T_min  0.6514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0825 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.8768.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.127
_exptl_crystal_description       platelet
_exptl_crystal_F_000             273.3
_exptl_crystal_size_max          0.056
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2843
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.125
_reflns_Friedel_fraction_full    0.281
_reflns_Friedel_fraction_max     0.155
_reflns_number_gt                1859
_reflns_number_total             2843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501486x_si_001.cif
_cod_data_source_block           NaVO2-xF2+x
_cod_depositor_comments
'Adding full bibliography for 4340863--4340864.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4340864
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Shared sites
{O2D, F2D}
{O6D, F6D}
2. Uiso/Uaniso restraints and constraints
Uanis(V2A) = Uanis(V2B)
Uanis(V1A) = Uanis(V1B)
Uanis(O4A) = Uanis(O4B)
Uanis(O8A) = Uanis(O8B)
Uanis(F5A) = Uanis(F5B)
Uanis(O2D) = Uanis(F2D)
Uanis(O6D) = Uanis(F6D)
Uanis(Na2B) = Uanis(Na2B)
Uanis(F7A) = Uanis(F7B)
3. Others
 Sof(V2B)=1-FVAR(1)
 Sof(V2A)=FVAR(1)
 Sof(V1B)=1-FVAR(2)
 Sof(V1A)=FVAR(2)
 Sof(O4B)=1-FVAR(3)
 Sof(O4A)=FVAR(3)
 Sof(O8B)=1-FVAR(4)
 Sof(O8A)=FVAR(4)
 Sof(F5B)=1-FVAR(5)
 Sof(F5A)=FVAR(5)
 Sof(F7B)=1-FVAR(6)
 Sof(F7A)=FVAR(6)
 Fixed Sof: F2D(0.33333) F6D(0.33333) O2D(0.66666) O6D(0.66666)
;