P-N/P-P Bond Metathesis for the Synthesis of Complex Polyphosphanes
Kai-Oliver Feldmann; Jan J. Weigand; Journal of the American Chemical Society 134 (2012) 15443–15456; doi:10.1021/ja305406x

data_4118626
_publ_contact_author_address
;
Institute of Inorganic and Analytical Chemistry
Westf\"alische Wilhelms-Universit\"at M\"unster
Corrensstr. 30
48149 M\"unster
;
_publ_contact_author_email       jweigand@uni-muenster.de
_publ_contact_author_fax         +49-251-8333126
_publ_contact_author_name        'Jan J. Weigand'
_publ_contact_author_phone       +49-251-8336074
_publ_section_title
;
 P-N/P-P Bond Metathesis for the Synthesis of Complex Polyphosphanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15443
_journal_page_last               15456
_journal_paper_doi               10.1021/ja305406x
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C42 H42 P8'
_chemical_formula_sum            'C42 H42 P8'
_chemical_formula_weight         794.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-05-23 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.958(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.1401(15)
_cell_length_b                   15.312(2)
_cell_length_c                   10.2692(12)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     2058.4(4)
_computing_cell_refinement       'APEX2 Software Suit (v2012.2-0)'
_computing_data_collection       'APEX2 Software Suit (v2012.2-0)'
_computing_data_reduction        'APEX2 Software Suit (v2012.2-0)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'HELIOS multilayer optics, Montel mirror'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14406
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.9503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.8588
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0544P)^2^+1.7175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                3097
_reflns_number_total             4864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305406x_si_003.cif
_cod_data_source_block           sada
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4118626