{μ~4~-3,3'-Bi[tricyclo[2.2.1.0^2,6^]heptaphosphane](4{-})}tetrakis[bis(1,2-dimethoxyethane)sodium(I)]
Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 63 (2007) m1013–m1014; doi:10.1107/S1600536807010100

data_2212889
_publ_section_title
{\m~4~-3,3'-Bi[tricyclo[2.2.1.0^2,6^]heptaphosphane](4{-})}tetrakis[bis(1,2-dimethoxyethane)sodium(I)]
_journal_coeditor_code           HB2311
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1013
_journal_page_last               m1014
_journal_paper_doi               10.1107/S1600536807010100
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Na4 (P14) (C4 H10 O2)8]'
_chemical_formula_moiety         'C32 H80 Na4 O16 P14'
_chemical_formula_sum            'C32 H80 Na4 O16 P14'
_chemical_formula_weight         1246.50
_chemical_name_systematic
;
{\m~4~-3,3'-Bi[tricyclo[2.2.1.0^2,6^]heptaphosphane](4-)}tetrakis[bis(1,2-
dimethoxyethane)sodium(I)]
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.444(2)
_cell_length_b                   20.264(3)
_cell_length_c                   12.874(2)
_cell_measurement_reflns_used    6420
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      3.5
_cell_volume                     3183.2(9)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  'SHELXL97 and PLATON'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Stoe IPDSII two-circle'
_diffrn_measurement_method       \w
_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  0.0897
_diffrn_reflns_av_sigmaI/netI    0.1855
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9106
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut needle'
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_gt           0.0682
_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^)+(0.02P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                2557
_reflns_number_total             5581
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2311.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212889
_cod_database_fobs_code          2212889