Structures and Unusual Rearrangements of Coordination Adducts of MX5 (M = Nb, Ta; X = F, Cl) with Simple Diethers. A Crystallographic, Spectroscopic, and Computational Study
Riccardo Bini; Cinzia Chiappe; Fabio Marchetti; Guido Pampaloni; Stefano Zacchini; Inorganic Chemistry 49 (2010) 339–351; doi:10.1021/ic9020806

data_4314494
_publ_section_title
;
 Structures and Unusual Rearrangements of Coordination Adducts of MX5 (M =
 Nb, Ta; X = F, Cl) with Simple Diethers. A Crystallographic,
 Spectroscopic, and Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              339
_journal_page_last               351
_journal_paper_doi               10.1021/ic9020806
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C8 H20 F10 O4 Ta2'
_chemical_formula_weight         732.14
_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                 118.920(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.650(5)
_cell_length_b                   12.719(5)
_cell_length_c                   12.671(5)
_cell_measurement_reflns_used    5729
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2615
_cell_measurement_theta_min      2.4365
_cell_volume                     1784.5(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1586
_diffrn_reflns_av_sigmaI/netI    0.1758
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14812
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    12.363
_exptl_absorpt_correction_T_max  0.3711
_exptl_absorpt_correction_T_min  0.2765
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.190
_refine_diff_density_min         -5.917
_refine_diff_density_rms         0.526
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3146
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0848
_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^)+(0.0652P)^2^+9.2330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.1927
_reflns_number_gt                2656
_reflns_number_total             3146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9020806_si_002_2.cif
_cod_data_source_block           tadme
_cod_original_cell_volume        1784.4(12)
_cod_database_code               4314494