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_4337527
_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         'C10 F5 N2 Nb1 O1'
_chemical_formula_sum            'C10 H10 F5 N2 Nb O'
_chemical_formula_weight         362.11
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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             2013-09-27T12:29:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9876(5)
_cell_length_b                   6.7669(3)
_cell_length_c                   14.1792(7)
_cell_measurement_reflns_used    3824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.5366
_cell_measurement_theta_min      7.3898
_cell_measurement_wavelength     0.71069
_cell_volume                     1150.20(9)
_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 0.98
_diffrn_measured_fraction_theta_max 0.98
_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      -0.702694E-1
_diffrn_orient_matrix_UB_12      0.267131E-2
_diffrn_orient_matrix_UB_13      -0.620013E-1
_diffrn_orient_matrix_UB_21      0.109854
_diffrn_orient_matrix_UB_22      0.457976E-1
_diffrn_orient_matrix_UB_23      -0.269467E-1
_diffrn_orient_matrix_UB_31      0.69516E-1
_diffrn_orient_matrix_UB_32      -0.696725E-1
_diffrn_orient_matrix_UB_33      -0.02009
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6511
_diffrn_reflns_theta_full        25.1
_diffrn_reflns_theta_max         25.1
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0014(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   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0195
_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^+1.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0519
_reflns_number_gt                940
_reflns_number_total             1004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402561g_si_004.cif
_cod_data_source_block           II
_cod_database_code               4337527