A “Push−Pull” Phosphasilene and Phosphagermene and Their Anion-Radicals
Lee, Vladimir Ya.; Kawai, Manami; Sekiguchi, Akira; Ranaivonjatovo, Henri; Escudié, Jean; Organometallics 28 (2009) 4262–; doi:10.1021/om900310u

data_4069627
_publ_section_title
;
 A &#x201C;Push&#x2212;Pull&#x201D; Phosphasilene and Phosphagermene and
 Their Anion-Radicals
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4262
_journal_paper_doi               10.1021/om900310u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C36 H71 Ge P Si2'
_chemical_formula_weight         663.67
_chemical_name_systematic
; 
 (t-Bu2MeSi)2Ge=P(2,4,6-t-Bu3-C6H2) 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7740(2)
_cell_length_b                   17.6480(5)
_cell_length_c                   19.4310(5)
_cell_measurement_reflns_used    40391
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.08
_cell_volume                     4037.52(17)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40391
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.307
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.539(16)
_refine_ls_extinction_coef       0.0104(11)
_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   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+7.7745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                4985
_reflns_number_total             5335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900310u_si_003.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 21 21    '
_cod_database_code               4069627