A Facile Synthesis of Diphosphasilacyclopropanes and 1,3-Diphospha-2,4-disilabicyclo[1.1.0]butanes and an ab Initio Study of Diphosphadisilabicyclo[1.1.0]butanes and Their Respective 1,3-Diene Isomers
Matthias Driess; Hans Pritzkow; Stefan Rell; Rudolf Janoschek; Inorganic Chemistry 36 (1997) 5212–5217; doi:10.1021/ic970580+

data_4327708
_publ_section_title
;
 A Facile Synthesis of Diphosphasilacyclopropanes and
 1,3-Diphospha-2,4-disilabicyclo[1.1.0]butanes and an ab Initio Study of
 Diphosphadisilabicyclo[1.1.0]butanes and Their Respective 1,3-Diene
 Isomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5212
_journal_page_last               5217
_journal_paper_doi               10.1021/ic970580+
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C65 H93 F P2 Si2'
_chemical_formula_weight         1011.51
_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, H at P2 difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 77.740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.847(3)
_cell_length_b                   22.559(5)
_cell_length_c                   21.071(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      3
_cell_volume                     6896(2)
_computing_cell_refinement       'P3 (Siemens)'
_computing_data_collection       'P3 (Siemens)'
_computing_data_reduction        'XDISK (Siemens)'
_computing_molecular_graphics    'ORTEP (C.Johnsson)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       omega-scan
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.1146
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10649
_diffrn_reflns_theta_max         23.51
_diffrn_reflns_theta_min         2.06
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.165
_refine_ls_hydrogen_treatment    'refU, H at P2 refall'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         10197
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.312
_refine_ls_R_factor_all          0.1847
_refine_ls_R_factor_obs          0.0859
_refine_ls_shift/esd_max         0.278
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+6.6217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2704
_refine_ls_wR_factor_obs         0.2062
_reflns_number_observed          4886
_reflns_number_total             10199
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9705802B_1.cif
_cod_data_source_block           drem
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+6.6217P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+6.6217P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6896.4(23)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4327708