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_4301295
_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            'C76 H158 Na2 O22 P4 Si2'
_chemical_formula_weight         1650.06
_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                 115.699(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.006(2)
_cell_length_b                   23.823(3)
_cell_length_c                   16.436(2)
_cell_measurement_reflns_used    10505
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.1
_cell_measurement_theta_min      2.2
_cell_volume                     5647.3(13)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_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  0.1731
_diffrn_reflns_av_sigmaI/netI    0.2097
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40944
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.9542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    0.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9929
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.351
_refine_ls_R_factor_all          0.3635
_refine_ls_R_factor_gt           0.2468
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5331
_refine_ls_wR_factor_ref         0.5762
_reflns_number_gt                3267
_reflns_number_total             9929
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic8016003_si_002.cif
_cod_data_source_block           wa487
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5647.3(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4301295