Alkynyl functionalized Al/P-based frustrated Lewis pairs - aluminium alkynide elimination and evidence for the formation of 3H-phosphaallenes [R-P[double bond, length as m-dash]C[double bond, length as m-dash]C(H)-(t)Bu].
Klöcker, Hans; Roters, Steffi; Hepp, Alexander; Uhl, Werner; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12670–12679; doi:10.1039/c5dt01607j

data_7035458
_publ_section_title
;
 Alkynyl functionalized Al/P-based frustrated Lewis pairs - aluminium
 alkynide elimination and evidence for the formation of 3H-phosphaallenes
 [R-P[double bond, length as m-dash]C[double bond, length as
 m-dash]C(H)-(t)Bu].
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12670
_journal_page_last               12679
_journal_paper_doi               10.1039/c5dt01607j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C38 H75 Al P Si4'
_chemical_formula_weight         702.29
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-21 deposited with the CCDC.
2015-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                96.6550(10)
_cell_angle_beta                 94.5070(10)
_cell_angle_gamma                110.3820(10)
_cell_formula_units_Z            2
_cell_length_a                   10.15150(10)
_cell_length_b                   11.79550(10)
_cell_length_c                   21.0988(2)
_cell_measurement_reflns_used    8934
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      72.637
_cell_measurement_theta_min      4.046
_cell_volume                     2333.01(4)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_laue_measured_fraction_full 0.875
_diffrn_reflns_laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13389
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.989
_diffrn_reflns_theta_min         2.126
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7379
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+0.7862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6747
_reflns_number_total             7379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01607j1.cif
_cod_data_source_block           sad1
_cod_depositor_comments
'Adding full bibliography for 7035458--7035461.cif.'
_cod_database_code               7035458
_shelx_estimated_absorpt_t_min   0.710
_shelx_estimated_absorpt_t_max   0.898
_shelxl_version_number           2013-4
_shelx_res_checksum              9790