Improving catalyst activity in secondary amine catalysed transformations.
Brazier, John B.; Gibbs, Timothy J. K.; Rowley, Julian H.; Samulis, Leopold; Yau, Sze Chak; Kennedy, Alan R.; Platts, James A.; Tomkinson, Nicholas C. O.; Organic & biomolecular chemistry 13 (2015) 133–141; doi:10.1039/c4ob01916d

data_7154141
_publ_section_title
;
 Improving catalyst activity in secondary amine catalysed transformations.
;
_journal_issue                   1
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              133
_journal_page_last               141
_journal_paper_doi               10.1039/c4ob01916d
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C29 H30 F6 I N3 O3.5 P'
_chemical_formula_weight         748.43
_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                86.399(4)
_cell_angle_beta                 86.024(4)
_cell_angle_gamma                73.657(4)
_cell_formula_units_Z            4
_cell_length_a                   10.4383(4)
_cell_length_b                   16.5706(7)
_cell_length_c                   18.8976(9)
_cell_measurement_reflns_used    9494
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.9553
_cell_measurement_theta_min      4.4169
_cell_volume                     3125.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25306
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         73.56
_diffrn_reflns_theta_min         4.42
_exptl_absorpt_coefficient_mu    9.185
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1500
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: ether'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.985
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         25307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+6.7582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1501
_reflns_number_gt                20007
_reflns_number_total             25307
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4ob01916d2.cif
_cod_data_source_block           tomp_jhr592
_cod_depositor_comments          'Adding full bibliography for 7154141.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C29 H30 F6 I N3 O3.50 P'
_cod_database_code               7154141