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_7035460
_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            'C21 H29 P'
_chemical_formula_weight         312.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1750(3)
_cell_length_b                   11.9208(4)
_cell_length_c                   16.3031(5)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.052
_cell_measurement_theta_min      2.36
_cell_volume                     1977.47(11)
_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 0.991
_diffrn_measured_fraction_theta_max 0.993
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15775
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.128
_diffrn_reflns_theta_min         2.359
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1904 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5233
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0660P)^2^+0.2880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.753
_reflns_friedel_fraction_full    0.987
_reflns_friedel_fraction_max     0.968
_reflns_number_gt                4801
_reflns_number_total             5233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01607j1.cif
_cod_data_source_block           sad2
_cod_depositor_comments
'Adding full bibliography for 7035458--7035461.cif.'
_cod_database_code               7035460
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2013-4
_shelx_res_checksum              80664