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_7005254
_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            'C31 H39 O9 P5 W2'
_chemical_formula_weight         1078.17
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.395(3)
_cell_length_b                   17.632(4)
_cell_length_c                   18.169(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3793.4(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12213
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    6.319
_exptl_absorpt_correction_T_max  0.570
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.707
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+7.0173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                6486
_reflns_number_total             8183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b618515k.txt
_cod_data_source_block           compound8
_cod_original_cell_volume        3793.4(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7005254