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_4116739
_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(hpp)4  2NaEt3BH'
_chemical_formula_sum            'C40 H80 B2 N12 Na2 Nb2'
_chemical_formula_weight         982.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 95.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.228(2)
_cell_length_b                   10.963(2)
_cell_length_c                   23.401(5)
_cell_measurement_reflns_used    194
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      6.5
_cell_volume                     2357.7(8)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        XPREP
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL-93
_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       'area detector'
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12648
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       needle
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.154
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_hydrogen_treatment    'calculated positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_obs          0.0356
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+4.9999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0909
_refine_ls_wR_factor_obs         0.0828
_reflns_number_observed          3560
_reflns_number_total             3982
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja980092g_3.cif
_cod_data_source_block           1.2NaEt3BH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+4.9999P] 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^)+(0.0262P)^2^+4.9999P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116739