Differing reactivities of P?CMe and P?CBut towards a triphosphabenzene and a tetraphosphabarrelene: synthesis of new phosphaalkyne pentamers (P5C5MenBut5?n, n = 0, 1 or 2)
Jones, Cameron; Schulten, Christian; Stasch, Andreas; Dalton Transactions  (2007) 1929–; doi:10.1039/b618515k

data_7005253
_publ_section_title
;
 Differing reactivities of P?CMe and P?CBut towards a triphosphabenzene
 and a tetraphosphabarrelene: synthesis of new phosphaalkyne pentamers
 (P5C5MenBut5?n, n = 0, 1 or 2)
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              1929
_journal_paper_doi               10.1039/b618515k
_journal_year                    2007
_chemical_formula_sum            'C29 H33 O10 P5 W2'
_chemical_formula_weight         1064.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.67(3)
_cell_angle_beta                 85.14(3)
_cell_angle_gamma                82.35(3)
_cell_formula_units_Z            2
_cell_length_a                   10.251(2)
_cell_length_b                   12.816(3)
_cell_length_c                   15.326(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1817.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21210
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    6.595
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.854
_refine_diff_density_min         -2.426
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0419P)^2^+3.3204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                5517
_reflns_number_total             6871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b618515k.txt
_cod_data_source_block           compound7
_cod_original_cell_volume        1817.3(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005253