Higher-Order Cyclopropenimine Superbases: Direct Neutral Brønsted Base Catalyzed Michael Reactions with α-Aryl Esters.
Nacsa, Eric D.; Lambert, Tristan H.; Journal of the American Chemical Society 137 (2015) 10246–10253; doi:10.1021/jacs.5b05033

data_4129447
_publ_section_title
;
 Higher-Order Cyclopropenimine Superbases: Direct Neutral Br\/onsted Base
 Catalyzed Michael Reactions with \a-Aryl Esters.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10246
_journal_page_last               10253
_journal_paper_doi               10.1021/jacs.5b05033
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C29 H58 N6 P, B F4'
_chemical_formula_sum            'C29 H58 B F4 N6 P'
_chemical_formula_weight         608.59
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_alpha                90
_cell_angle_beta                 108.269(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   14.832(2)
_cell_length_c                   19.373(3)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.21
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_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.501
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_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  .7461
_exptl_absorpt_correction_T_min  .6043
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     385
_refine_ls_number_reflns         9935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0553P)^2^+4.0633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.000
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_reflns_number_total             9935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05033_si_006.cif
_cod_data_source_block           phosphinimine
_cod_original_cell_volume        3400.3(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4129447
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              98
_shelx_hkl_checksum              2495