Synthesis, Crystal Structure, and Characterization of the First Nb3 Triangular Cluster Compound Bonded to Fluorine Ligands: Association of Nb3IiFi3Fa8La Units and NbIVL6 Octahedra with L = O and F
S. Cordier; O. Hernandez; J.-Y. Thépot; A. I. Shames; C. Perrin; Inorganic Chemistry 42 (2003) 1101–1106; doi:10.1021/ic025667w

data_4313138
_publ_contact_author_address
;
LCSIM UMR 6511 CNRS - Universit\'e de Rennes 1, Institut de Chimie
de Rennes, B\^at. 10A, Campus de Beaulieu, Avenue du G\'en\'eral Leclerc,
35042 Rennes, France
;
_publ_contact_author_email       stephane.cordier@univ-rennes1.fr
_publ_contact_author_fax         '33 2 23 23 65 36'
_publ_contact_author_name        'Stephane Cordier'
_publ_contact_author_phone       '33 2 99 63 57 04'
_publ_section_title
;
 Synthesis, Crystal Structure, and Characterization of the First Nb3
 Triangular Cluster Compound Bonded to Fluorine Ligands: Association of
 Nb3IiFi3Fa8La Units and NbIVL6 Octahedra with L = O and F
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1101
_journal_page_last               1106
_journal_paper_doi               10.1021/ic025667w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'F8.32 I1.00 Nb3.25 O0.18'
_chemical_formula_sum            'F8.32 I Nb3.25 O0.18'
_chemical_formula_weight         589.797
_chemical_name_systematic        ?
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8638(3)
_cell_length_b                   13.8638(3)
_cell_length_c                   8.9183(2)
_cell_measurement_reflns_used    10130
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      1.00
_cell_volume                     1714.14(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 1999)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1999)
;
_computing_publication_material
;
CRYSTALS Issue 11 (Watkin et al., 1999)
;
_computing_structure_refinement
;
CRYSTALS Issue 11 (Watkin et al., 1999)
;
_computing_structure_solution    'SIR97 (Cascarano et al., 1996)'
_diffrn_ambient_temperature      293(1)
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19223
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         1.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.95
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
from symmetry-related measurements (Blessing, 1995)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.572
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2100.56
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.14
_refine_diff_density_min         -1.08
_refine_ls_extinction_coef       14(1)
_refine_ls_extinction_method
;
Larson 1970 Crystallographic Computing eq 22
;
_refine_ls_goodness_of_fit_ref   1.0935
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1048
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.007424
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979,
0.567    0.369    0.609    0.110    0.255
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0244
_reflns_number_gt                1048
_reflns_number_total             1991
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ic025667w-2_si.cif
_cod_data_source_block           nbifo293
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_formula_sum        'F8.32 I1.00 Nb3.25 O0.18'
_cod_database_code               4313138