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_4308581
_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 Cu F5 N8 Nb O'
_chemical_formula_weight         643.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 109.270(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8224(14)
_cell_length_b                   16.385(3)
_cell_length_c                   8.9020(14)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.49
_cell_volume                     1214.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10966
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.9803
_exptl_absorpt_correction_type   'face indexed'
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      1.731(3)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       needle
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.5259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                2090
_reflns_number_total             2880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048766dsi20040903_031408_3.cif
_cod_data_source_block           Cu(3-apy)4NbOF5
_cod_original_cell_volume        1214.7(3)
_cod_database_code               4308581