The frustrated Lewis pair pathway to methylene phosphonium systems
Hasegawa, Yasuharu; Kehr, Gerald; Ehrlich, Stephan; Grimme, Stefan; Daniliuc, Constantin G.; Erker, Gerhard; Chemical Science 5 (2014) 797–; doi:10.1039/c3sc52327f

data_1513650
_publ_section_title
;
 The frustrated Lewis pair pathway to methylene phosphonium systems
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              797
_journal_paper_doi               10.1039/c3sc52327f
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C39 H41 B F10 N P'
_chemical_formula_weight         755.51
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.350(2)
_cell_angle_beta                 96.684(6)
_cell_angle_gamma                111.631(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8542(5)
_cell_length_b                   13.8552(5)
_cell_length_c                   14.0717(10)
_cell_measurement_reflns_used    6064
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1876.71(19)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26113
_diffrn_reflns_theta_full        67.02
_diffrn_reflns_theta_max         67.02
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.9608
_exptl_absorpt_correction_T_min  0.7475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         6459
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0554
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+1.0884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                5426
_reflns_number_total             6459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52327f.txt
_cod_data_source_block           erk6882
_cod_original_cell_volume        1876.71(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513650