A Solid-State NMR, X-ray Diffraction, and Ab Initio Investigation into the Structures of Novel Tantalum Oxyfluoride Clusters
Alam, Todd M.; Clawson, Jacalyn S.; Bonhomme, François; Thoma, Steven G.; Rodriguez, Mark A.; Zheng, Shaohui; Autschbach, Jochen; Chemistry of Materials 20 (2008) 2205–; doi:10.1021/cm0717763

data_4001088
_publ_section_title
;
 A Solid-State NMR, X-ray Diffraction, and Ab Initio Investigation into
 the Structures of Novel Tantalum Oxyfluoride Clusters
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2205
_journal_paper_doi               10.1021/cm0717763
_journal_volume                  20
_journal_year                    2008
_chemical_formula_moiety         'Ta4 F16 O4, 4(C5 N H6)'
_chemical_formula_sum            'C20 H24 F16 N4 O4 Ta4'
_chemical_formula_weight         1412.24
_chemical_name_common            TAF16-PYR
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/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                 92.327(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0476(12)
_cell_length_b                   15.897(2)
_cell_length_c                   10.8230(15)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.28
_cell_volume                     1555.4(4)
_computing_cell_refinement       'SMART 5.054 (Bruker, 1998)'
_computing_data_collection       'SMART 5.054 (Bruker, 1998)'
_computing_data_reduction        'SAINT 6.02 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 5.1  (Bruker, 1998)'
_computing_publication_material  'SHELXTL 5.1  (Bruker, 1998)'
_computing_structure_refinement  'XSHELL 4.01 (Bruker, 2000)'
_computing_structure_solution    'SHELXTL 5.1  (Bruker, 1998)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4079
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.154
_exptl_absorpt_correction_T_max  0.3318
_exptl_absorpt_correction_T_min  0.1641
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick (1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.145
_refine_diff_density_min         -2.205
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1428
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0077P)^2^+89.8807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                1362
_reflns_number_total             1428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm0717763-file004.cif
_cod_data_source_block           TAF16PYR
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     '-I 2y '
_cod_original_sg_symbol_H-M      'I2/m  '
_cod_database_code               4001088