Intriguing Tetrasodium Dication Cluster Na42+ Stabilized between Two Silyl(fluorosilyl)phosphanide Shells
Matthias Driess; Hans Pritzkow; Markus Skipinski; Uwe Winkler; Journal of the American Chemical Society 120 (1998) 10774–10775; doi:10.1021/ja9822963

data_4116855
_publ_contact_author
;
        Klaus Merz
Lehrstuhl fuer Anorganische Chemie 1
Ruhr-Universitaet Bochum
Universitaetsstrasse 150
D-44780 Bochum
Deutschland
;
_publ_contact_author_fax         '049 234 709-4378'
_publ_contact_author_phone       '049 234 700-4154'
_publ_section_title
;
 Intriguing Tetrasodium Dication Cluster Na42+ Stabilized between Two
 Silyl(fluorosilyl)phosphanide Shells
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10774
_journal_page_last               10775
_journal_paper_doi               10.1021/ja9822963
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C78 H134 F2 Na4 P2 Si4'
_chemical_formula_weight         1376.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.78(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.919(6)
_cell_length_b                   26.140(14)
_cell_length_c                   15.057(8)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      11.8
_cell_volume                     4191(4)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'ORTEP (C.K.Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Siemens-Stoe AED2'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0799
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_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7201
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7201
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+0.2797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                4131
_reflns_number_total             7201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9822963.cif
_cod_data_source_block           uw100
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+0.2797P] 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^)+(0.0868P)^2^+0.2797P] where P=(Fo^2^+2Fc^2^)/3'.

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

2024-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C39 H67 F Na2 P Si2'
_cod_original_formula_weight         688.06
_cod_original_formula_units_Z            4
_cod_database_code               4116855