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_4327709
_publ_section_title
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 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
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_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            'C77 H123 F Li O3 P2 Si2'
_chemical_formula_weight         1240.81
_chemical_name_systematic
;
 ?
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_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.88(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.845(11)
_cell_length_b                   24.594(19)
_cell_length_c                   21.132(16)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      5
_cell_volume                     7698(10)
_computing_cell_refinement       'DIF4 (Siemens-Stoe)'
_computing_data_collection       'DIF4 (Siemens-Stoe)'
_computing_data_reduction        'REDU4 (Siemens-Stoe)'
_computing_molecular_graphics    'ORTEP (C.K.Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens-Stoe AED2'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1498
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10145
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        7
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_F_000             2716
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.3
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         10143
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.024
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.1832
_refine_ls_R_factor_obs          0.0767
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+6.9812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2064
_refine_ls_wR_factor_obs         0.1590
_reflns_number_observed          5243
_reflns_number_total             10145
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9705802B_2.cif
_cod_data_source_block           ma57
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+6.9812P] 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^)+(0.0741P)^2^+6.9812P] 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        7697.6(101)
_cod_database_code               4327709