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_4323411
_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            'C40 H80 Cl8 Mg Nb2 O12'
_chemical_formula_weight         1246.77
_chemical_name_systematic
;
trans-[bis(*-O){trans-tetrachloro-tetrahydrofuran-niobium(V)}]-tetrakis(tetra-
hydrofuran)-magnesium dichloromethane(1/1)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.97(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.943(4)
_cell_length_b                   13.365(3)
_cell_length_c                   26.488(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      10
_cell_volume                     5845(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            1453
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         1414
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0435
_refine_ls_shift/esd_max         -0.037
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+10.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1141
_refine_ls_wR_factor_obs         0.1141
_reflns_number_observed          1414
_reflns_number_total             1414
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9610804_1.cif
_cod_data_source_block           compund_1_[{bOCl4(THF)}2(Mg(THF)4)CH2Cl2]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+10.0790P] 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^)+(0.0827P)^2^+10.0790P] 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        5845.0(23)
_cod_database_code               4323411