A retro diels-alder route to diphosphorus chemistry: molecular precursor synthesis, kinetics of p2 transfer to 1,3-dienes, and detection of p2 by molecular beam mass spectrometry.
Velian, Alexandra; Nava, Matthew; Temprado, Manuel; Zhou, Yan; Field, Robert W.; Cummins, Christopher C.; Journal of the American Chemical Society 136 (2014) 13586–13589; doi:10.1021/ja507922x

data_4122641
_publ_section_title
;
 A retro diels-alder route to diphosphorus chemistry: molecular precursor
 synthesis, kinetics of p2 transfer to 1,3-dienes, and detection of p2 by
 molecular beam mass spectrometry.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13586
_journal_page_last               13589
_journal_paper_doi               10.1021/ja507922x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C29.5 H23 Al2 Cl8 P2'
_chemical_formula_weight         776.98
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.900(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5027(10)
_cell_length_b                   21.598(2)
_cell_length_c                   14.9821(14)
_cell_measurement_temperature    100(2)
_cell_volume                     3284.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            68597
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.9267
_exptl_absorpt_correction_T_min  0.5845
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         9978
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0856
_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^)+(0.0577P)^2^+20.2879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.2251
_reflns_number_gt                7853
_reflns_number_total             9978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            P2A2ClAlCl4.cif
_cod_data_source_block           x8_13048_final
_cod_depositor_comments
'Adding full bibliography for 4122640--4122642.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C29.50 H23 Al2 Cl8 P2'
_cod_database_code               4122641