From solution to the solid state: control of niobium oxide-fluoride [NbOxFy]n- species.
Lu, Hongcheng; Gautier, Romain; Donakowski, Martin D.; Liu, Zhengtang; Poeppelmeier, Kenneth R.; Inorganic chemistry 53 (2014) 537–542; doi:10.1021/ic402561g

data_4337526
_publ_section_title
;
 From solution to the solid state: control of niobium oxide-fluoride
 [NbOxFy]n- species.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              537
_journal_page_last               542
_journal_paper_doi               10.1021/ic402561g
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'F4 Nb O, 2(C2.5 H3 N0.5)'
_chemical_formula_sum            'C5 H6 F4 N Nb O'
_chemical_formula_weight         265.06
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-04-13T19:54:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.464(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.9511(4)
_cell_length_b                   14.0715(17)
_cell_length_c                   7.0890(9)
_cell_measurement_reflns_used    635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.5532
_cell_measurement_theta_min      2.8786
_cell_measurement_wavelength     0.71073
_cell_volume                     393.41(8)
_computing_cell_refinement       'SAINT V7.68A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      -0.165712E-1
_diffrn_orient_matrix_UB_12      0.69772E-1
_diffrn_orient_matrix_UB_13      0.245975E-1
_diffrn_orient_matrix_UB_21      -0.195577E-1
_diffrn_orient_matrix_UB_22      0.12309E-1
_diffrn_orient_matrix_UB_23      -0.139163
_diffrn_orient_matrix_UB_31      -0.252258
_diffrn_orient_matrix_UB_32      -0.553774E-2
_diffrn_orient_matrix_UB_33      0.589747E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.1206
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10757
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    1.55
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.051
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.97
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                739
_reflns_number_total             1192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402561g_si_004.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C5 H6 F4 N1 Nb O'
_cod_database_code               4337526