Structural Studies of Indium and Thallium Insertion into the Framework of the Cluster Compound Ti2Nb6Cl14O4
Ekaterina Anokhina; Michael Essig; Cynthia Day; Abdessadek Lachgar; Inorganic Chemistry 39 (2000) 2185–2188; doi:10.1021/ic9913536

data_4320953
_publ_contact_author_address
;
    Department of Chemistry, 
    Wake Forest University, 
    Winston-Salem, NC 27109 USA
;
_publ_contact_author_email       lachgar@wfu.edu
_publ_contact_author_fax         '(336) 758-4656'
_publ_contact_author_name        'Abdessadek Lachgar'
_publ_contact_author_phone       '(336) 758-4676'
_publ_section_title
;
 Structural Studies of Indium and Thallium Insertion into the Framework of
 the Cluster Compound Ti2Nb6Cl14O4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2185
_journal_page_last               2188
_journal_paper_doi               10.1021/ic9913536
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'Cl13.8 Nb6 O4.2 Ti2 Tl0.2'
_chemical_formula_weight         1250.54
_chemical_name_systematic
; 
 ? 
;
_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-97 and manual editing of form.cif'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.277(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7319(14)
_cell_length_b                   14.6069(19)
_cell_length_c                   12.6624(19)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.08
_cell_measurement_theta_min      2.75
_cell_volume                     2344.9(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ATOMS for Windows'
_computing_publication_material  'Bruker SHELXTL'
_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  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3697
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.416
_exptl_absorpt_correction_T_max  0.6328
_exptl_absorpt_correction_T_min  0.5223
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2298
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                2323
_reflns_number_total             3041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9913536_1.cif
_cod_data_source_block           tl020
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'Cl13.80 Nb6 O4.20 Ti2 Tl0.20'
_cod_database_code               4320953