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_4129443
_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         'C37 H66 N7, B F4'
_chemical_formula_sum            'C37 H66 B F4 N7'
_chemical_formula_weight         695.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 98.735(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.235(3)
_cell_length_b                   15.647(3)
_cell_length_c                   16.426(3)
_cell_measurement_temperature    130(2)
_cell_volume                     4124.3(13)
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.9944
_diffrn_measured_fraction_theta_max 0.9944
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            64922
_diffrn_reflns_theta_full        30.5221
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5271
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.1205
_exptl_crystal_F_000             1512.6899
_exptl_crystal_size_max          1.300
_exptl_crystal_size_mid          1.100
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.4969
_refine_diff_density_min         -0.4613
_refine_diff_density_rms         0.0767
_refine_ls_d_res_high            0.6997
_refine_ls_d_res_low             12.3924
_refine_ls_goodness_of_fit_ref   1.1312
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    93
_refine_ls_number_parameters     462
_refine_ls_number_reflns         12540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1312
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.0153
_refine_ls_shift/su_mean         0.0014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1813
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -23
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -14
_reflns_number_gt                8758
_reflns_number_total             12540
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja5b05033_si_005.cif
_cod_data_source_block           s-Copy
_cod_original_cell_volume        4124.3(14)
_cod_database_code               4129443
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  {H37a,H37b} of C37, {H36a,H36b} of C36, H27 of C27, H14 of C14, H29 of C29, 
  H24 of C24, {H35a,H35b} of C35, H18 of C18, H33 of C33, H11 of C11, H7 of C7 
 At 1.5 times of: 
  {H10a,H10b,H10c} of C10, {H38a,H38b,H38c} of C38, {H13a,H13b,H13c} of C13, 
  {H19a,H19b,H19c} of C19, {H17a,H17b,H17c} of C17, {H34a,H34b,H34c} of C34, 
  {H16a,H16b,H16c} of C16, {H23a,H23b,H23c} of C23, {H26a,H26b,H26c} of C26, 
  {H28a,H28b,H28c} of C28, {H25a,H25b,H25c} of C25, {H31a,H31b,H31c} of C31, 
  {H12a,H12b,H12c} of C12, {H8a,H8b,H8c} of C8, {H32a,H32b,H32c} of C32, {H30a, 
  H30b,H30c} of C30, {H15a,H15b,H15c} of C15 
2.a Ternary CH refined with riding coordinates: 
 C7(H7), C11(H11), C33(H33), C18(H18), C24(H24), C29(H29), C14(H14), C27(H27) 
2.b Secondary CH2 refined with riding coordinates: 
 C35(H35a,H35b), C36(H36a,H36b), C37(H37a,H37b) 
2.c Idealised Me refined as rotating group: 
 C32(H32a,H32b,H32c), C8(H8a,H8b,H8c), C12(H12a,H12b,H12c), C31(H31a,H31b, 
 H31c), C25(H25a,H25b,H25c), C10(H10a,H10b,H10c), C26(H26a,H26b,H26c), C23(H23a, 
 H23b,H23c), C16(H16a,H16b,H16c), C34(H34a,H34b,H34c), C17(H17a,H17b,H17c), 
 C19(H19a,H19b,H19c), C28(H28a,H28b,H28c), C13(H13a,H13b,H13c), C30(H30a,H30b, 
 H30c), C15(H15a,H15b,H15c), C38(H38a,H38b,H38c) 
;