Examining the Out-of-Center Distortion in the [NbOF5]2- Anion
Heather K. Izumi; Janet E. Kirsch; Charlotte L. Stern; Kenneth R. Poeppelmeier; Inorganic Chemistry 44 (2005) 884–895; doi:10.1021/ic048766d

data_4308580
_publ_section_title
;
Examining the Out-of-Center Distortion in the [NbOF5]2- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              884
_journal_page_last               895
_journal_paper_doi               10.1021/ic048766d
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C20 H24 Cd F5 N8 Nb O'
_chemical_formula_weight         692.78
_chemical_name_common            Cd(C~5~H~6~N~2~)~4~NbOF~5~
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4034(4)
_cell_length_b                   8.4034(4)
_cell_length_c                   34.933(3)
_cell_measurement_reflns_used    6993
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.42
_cell_volume                     2466.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type
;
Bruker SMART 1000 CCD area detector diffractometer
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            23209
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  0.8943
_exptl_absorpt_correction_T_min  0.6461
_exptl_absorpt_correction_type   'face indexed'
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_meas      1.884(8)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6078
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+6.0806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                5555
_reflns_number_total             6078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048766dsi20040903_031408_2.cif
_cod_data_source_block           Cd(3-apy)4NbOF5
_cod_original_cell_volume        2466.9(2)
_cod_database_code               4308580