Synthesis and structure of a tetranuclear niobium telluride cuboidal cluster with a central μ4-O ligand
Fedin, Vladimir P.; Kalinina, Irina V.; Virovets, Alexander V.; Podberezskaya, Nina V.; Neretin, Ivan S.; Slovokhotov, Yuri L.; Chemical Communications  (1998) 2579–; doi:10.1039/a805956j

data_7110356
_publ_section_title
;
 Synthesis and structure of a tetranuclear niobium telluride cuboidal
 cluster with a central \m4-O ligand
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2579
_journal_paper_doi               10.1039/a805956j
_journal_year                    1998
_chemical_formula_moiety
'K6 [Nb4 Te4 O (C N)12] . K2 C O3 . K O H . 8(H2 O)'
_chemical_formula_sum            'C13 H17 K9 N12 Nb4 O13 Te4'
_chemical_formula_weight         1783.33
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 91.584(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4688(9)
_cell_length_b                   22.658(4)
_cell_length_c                   16.318(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.2
_cell_measurement_theta_min      9.0
_cell_volume                     4608.4(10)
_computing_cell_refinement       'CD4CA0 CAD4 Program'
_computing_data_collection       'CD4CA0 CAD4 Program'
_computing_data_reduction        XCAD
_computing_molecular_graphics    'ORTEP II'
_computing_publication_material  'manual edditing of CIF file'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       theta/2theta
_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  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8724
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '3600 sec'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.325
_exptl_absorpt_correction_T_max  0.56291
_exptl_absorpt_correction_T_min  0.29417
_exptl_absorpt_correction_type   'integration from crystal shape'
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.570
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       0.00020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1347
_reflns_number_gt                5272
_reflns_number_total             8316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            805956jsup1.cif
_cod_data_source_block           Nb4OTe4CN12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'nonr' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4608(1)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7110356