Triply Bonded Nb24+ Tetragonal Lantern Compounds: Some Accompanied by Novel B-H...Na+ Interactions
F. Albert Cotton; John H. Matonic; Carlos A. Murillo; Journal of the American Chemical Society 120 (1998) 6047–6052; doi:10.1021/ja980092g

data_4116737
_publ_contact_author_email       Cotton@tamu.edu
_publ_contact_author_phone       (409)-845-1533
_publ_section_title
;
 Triply Bonded Nb24+ Tetragonal Lantern Compounds: Some Accompanied by
 Novel B-H...Na+ Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6047
_journal_page_last               6052
_journal_paper_doi               10.1021/ja980092g
_journal_volume                  120
_journal_year                    1998
_chemical_formula_structural     'Nb2(N2C7H5)4 2LiCl 4THF'
_chemical_formula_sum            'C48 H48 Cl2 Li2 N8 Nb2 O2'
_chemical_formula_weight         1039.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.100(2)
_cell_length_b                   14.100(2)
_cell_length_c                   11.614(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      9
_cell_volume                     2309.0(6)
_computing_cell_refinement       'MADNES, (NONIUS, 1994)'
_computing_data_collection       'MADNES, (NONIUS, 1994)'
_computing_data_reduction        'XPREP (Sheldrick, 1993)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material  'SHELXTL (Sheldrick, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       'fitted profile from frame data'
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4880
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   Sortav
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       needle
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(20)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.147
_refine_ls_goodness_of_fit_obs   1.138
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_obs          0.0517
_refine_ls_shift/esd_max         0.218
_refine_ls_shift/esd_mean        0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+16.7959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1386
_refine_ls_wR_factor_obs         0.1272
_reflns_number_observed          1334
_reflns_number_total             1508
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja980092g_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+16.7959P] 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^)+(0.0486P)^2^+16.7959P] 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        2309.1(7)
_cod_database_code               4116737