Synthesis and Molecular Structures of the Magnesium and Aluminum Adducts of a Niobium-Oxo Complex. X-ray Crystal Structures of [{NbOCl4(THF)}2Mg(THF)4] and [{NbOCl4(THF)}2AlCl(THF)3]
Piotr Sobota; Józef Utko; Sławomir Szafert; Inorganic Chemistry 36 (1997) 2227–2229; doi:10.1021/ic9610804

data_4323413
_publ_section_title
;
 Synthesis and Molecular Structures of the Magnesium and Aluminum Adducts
 of a Niobium-Oxo Complex. X-ray Crystal Structures of
 [{NbOCl4(THF)}2Mg(THF)4] and [{NbOCl4(THF)}2AlCl(THF)3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2227
_journal_page_last               2229
_journal_paper_doi               10.1021/ic9610804
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C20 H40 Al Cl9 Nb2 O7'
_chemical_formula_weight         924.37
_chemical_name_systematic
;
trans-[bis(*-O){trans-tetrachloro-tetrahydrofuran-niobium(V)}]-
tris(tetrahydrofuran)chloroaluminium]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                67.17(3)
_cell_angle_beta                 78.70(2)
_cell_angle_gamma                65.03(3)
_cell_formula_units_Z            2
_cell_length_a                   12.051(3)
_cell_length_b                   13.794(4)
_cell_length_c                   14.948(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    300(1)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      10
_cell_volume                     2074.6(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(1)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4365
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.183
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_obs          0.0377
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+3.7456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1009
_refine_ls_wR_factor_obs         0.1009
_reflns_number_observed          4313
_reflns_number_total             4313
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9610804_3.cif
_cod_data_source_block           compund_3_[{NbOCl4(THF)}2(AlCl3(THF)3)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+3.7456P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+3.7456P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2074.6(10)
_cod_database_code               4323413