Structural Characterization and Dynamic Solution Behavior of the Disodio and Lithio−Sodio Geminal Organodimetallics [{{Ph2P(Me3Si)N}2CNa2}2] and [{{Ph2P(Me3Si)N}2CLiNa}2]
Hull, Katherine L.; Noll, Bruce C.; Henderson, Kenneth W.; Organometallics 25 (2006) 4072–; doi:10.1021/om0605635

data_4074343
_publ_section_title
;
 Structural Characterization and Dynamic Solution Behavior of the Disodio
 and Lithio&#x2212;Sodio Geminal Organodimetallics
 [{{Ph2P(Me3Si)N}2CNa2}2] and [{{Ph2P(Me3Si)N}2CLiNa}2]
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4072
_journal_paper_doi               10.1021/om0605635
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C62 H76 Li2 N4 Na2 P4 Si4, 2(C6 H6)'
_chemical_formula_sum            'C74 H88 Li2 N4 Na2 P4 Si4'
_chemical_formula_weight         1329.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.530(3)
_cell_angle_beta                 105.048(2)
_cell_angle_gamma                104.295(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5700(6)
_cell_length_b                   14.5952(6)
_cell_length_c                   18.6933(8)
_cell_measurement_reflns_used    9721
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0895
_cell_measurement_theta_min      2.2671
_cell_volume                     3702.4(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-ApexII CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            300720
_diffrn_reflns_theta_full        37.23
_diffrn_reflns_theta_max         37.23
_diffrn_reflns_theta_min         1.13
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.9539
_exptl_absorpt_correction_T_min  0.9377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G. M. (2005) SADABS. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method 'cooling from hot benzene solution'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         38148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+1.6369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                24855
_reflns_number_total             38148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0605635si20060627_102851.cif
_cod_data_source_block           klh03_0m
_cod_database_code               4074343