Supersilylated Tetraphosphene Derivatives M2[t-Bu3SiPPPPSi-t-Bu3] (M = Li, Na, Rb, Cs) and Ba[t-Bu3SiPPPPSi-t-Bu3]: Reactivity and Cis-Trans Isomerization
Andreas Lorbach; Andor Nadj; Sandor Tüllmann; Franz Dornhaus; Frauke Schödel; Inge Sänger; Günter Margraf; Jan W. Bats; Michael Bolte; Max C. Holthausen; Matthias Wagner; Hans-Wolfram Lerner; Inorganic Chemistry 48 (2009) 1005–1017; doi:10.1021/ic8016003

data_4301294
_publ_section_title
;
Supersilylated Tetraphosphene Derivatives M2[t-Bu3SiPPPPSi-t-Bu3] (M = Li,
Na, Rb, Cs) and Ba[t-Bu3SiPPPPSi-t-Bu3]: Reactivity and Cis-Trans
Isomerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1005
_journal_page_last               1017
_journal_paper_doi               10.1021/ic8016003
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C24 H54 I2 P4 Si2'
_chemical_formula_weight         776.53
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 90.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.226(5)
_cell_length_b                   8.4316(8)
_cell_length_c                   26.135(8)
_cell_measurement_reflns_used    71
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     3355.1(15)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  SIEMENS_SMART_CCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0951
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            28691
_diffrn_reflns_theta_full        32.24
_diffrn_reflns_theta_max         32.24
_diffrn_reflns_theta_min         0.78
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  600
_diffrn_standards_number         426
_exptl_absorpt_coefficient_mu    2.150
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   'empirical, SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.196
_refine_diff_density_min         -2.057
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.00106(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.06P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                4146
_reflns_number_total             5333
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic8016003_si_001.cif
_cod_data_source_block           margraf13
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4301294