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_4308579
_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            'C30 H38 Cu F10 N12 Nb2 O2'
_chemical_formula_weight         1038.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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            8
_cell_length_a                   20.8745(8)
_cell_length_b                   20.8745(8)
_cell_length_c                   17.2929(9)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.48
_cell_volume                     7535.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33069
_diffrn_reflns_theta_full        28.94
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.9397
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   'face indexed'
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      1.83(7)
_exptl_crystal_density_method    'flotation pycnometry'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.438
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.165
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+20.4668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                1913
_reflns_number_total             2436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048766dsi20040903_031408_1.cif
_cod_data_source_block           '[4-apyH][Cu(4-apy)4(NbOF5)2]'
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4308579