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_7035461
_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            'C37 H74 Al P Si4'
_chemical_formula_weight         689.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 111.670(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4546(16)
_cell_length_b                   13.0416(11)
_cell_length_c                   20.2605(17)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.44
_cell_volume                     4531.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60167
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.971
_diffrn_reflns_theta_min         1.962
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6265
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.330
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10869
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+1.6958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9142
_reflns_number_total             10869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01607j1.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7035458--7035461.cif.'
_cod_database_code               7035461
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-4
_shelx_res_checksum              98164