Phospha-Claisen Type Reactions at Frustrated Lewis Pair Frameworks.
Chen, Guo-Qiang; Kehr, Gerald; Mück-Lichtenfeld, Christian; Daniliuc, Constantin G.; Erker, Gerhard; Journal of the American Chemical Society 138 (2016) 8554–8559; doi:10.1021/jacs.6b04046

data_4130487
_publ_section_title
;
 Phospha-Claisen Type Reactions at Frustrated Lewis Pair Frameworks.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8554
_journal_page_last               8559
_journal_paper_doi               10.1021/jacs.6b04046
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C41 H36 B F10 O4 P'
_chemical_formula_weight         824.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                65.606(2)
_cell_angle_beta                 70.053(2)
_cell_angle_gamma                77.352(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3650(5)
_cell_length_b                   14.8236(7)
_cell_length_c                   16.1305(7)
_cell_measurement_reflns_used    5798
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.4195
_cell_measurement_theta_min      2.3304
_cell_volume                     2316.74(19)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;
APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)

;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16994
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.33
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.099
_platon_squeeze_details
;
Two badly disordered dichloromethane molecules were found in the
asymmetrical unit and could not be satisfactorily refined. The program 
SQUEEZE (A. L. Spek J. Appl. Cryst., 2003, 36, 7-13) was therefore used
to remove mathematically the effect of the solvent. 
The quoted formula and derived parameters are not included the squeezed
solvent molecules. 
;
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0943P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                5669
_reflns_number_total             8176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04046_si_003.cif
_cod_data_source_block           erk7994
_cod_database_code               4130487
_shelx_res_checksum              21425
_shelx_hkl_checksum              68591