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_4340863
_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         'F4 H2 O2 V, Na'
_chemical_formula_sum            'F4 H2 Na O2 V'
_chemical_formula_weight         183.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9595(4)
_cell_length_b                   9.4423(3)
_cell_length_c                   4.8186(2)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.365
_cell_measurement_theta_min      2.973
_cell_volume                     453.14(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0240
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            17392
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.501
_diffrn_reflns_theta_min         2.973
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.285
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0619 before and 0.0429 after correction.
The Ratio of minimum to maximum transmission is 0.8671.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.696
_exptl_crystal_description       platelet
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 663 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.039(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1511
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0121
_refine_ls_R_factor_gt           0.0117
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+0.0516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0326
_refine_ls_wR_factor_ref         0.0329
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1489
_reflns_number_total             1511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501486x_si_002.cif
_cod_data_source_block           navof4(h2o)
_cod_depositor_comments
'Adding full bibliography for 4340863--4340864.cif.'
_cod_database_code               4340863
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.643
_olex2_refinement_description
;
;