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_4129444
_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_sum            'C34 H68 B2 F8 N14'
_chemical_formula_weight         846.64
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.8374(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4197(9)
_cell_length_b                   11.8959(8)
_cell_length_c                   30.718(2)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.65
_cell_measurement_theta_min      2.45
_cell_volume                     4536.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            72998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.658
_diffrn_reflns_theta_min         1.326
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6762
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.850
_exptl_crystal_size_mid          0.810
_exptl_crystal_size_min          0.510
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         13974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+2.2689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11695
_reflns_number_total             13974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05033_si_002.cif
_cod_data_source_block           s
_cod_original_cell_volume        4536.0(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129444
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.951
_shelxl_version_number           2013-4
_shelx_res_checksum              4259
_shelx_hkl_checksum              82860