Molecular Recognition of Aliphatic Diamines by 3,3'-Di(trifluoroacetyl)-1,1'-bi-2-naphthol
Shanshan Yu; Winston Plunkett; Michael Kim; Elaine Wu; Michal Sabat; Lin Pu; Journal of Organic Chemistry 78 (2013) 12671–12680; doi:10.1021/jo402277p

data_4028879
_publ_section_title
;
 Molecular Recognition of Aliphatic Diamines by
 3,3'-Di(trifluoroacetyl)-1,1'-bi-2-naphthol
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              12671
_journal_page_last               12680
_journal_paper_doi               10.1021/jo402277p
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C28 H24 F6 N4 O2'
_chemical_formula_weight         562.51
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.532(3)
_cell_length_b                   10.532(3)
_cell_length_c                   44.888(12)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      3.55
_cell_volume                     4979(2)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_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  0.0647
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            47263
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.819
_diffrn_reflns_theta_min         3.283
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5316
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
; 
 Flack x determined using 4089 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_coef       0.0008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         9416
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+25.7119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2137
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                9007
_reflns_number_total             9416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo402277p_si_002_2.cif
_cod_data_source_block           C28H24F6N4O2
_cod_original_cell_volume        4979(3)
_cod_database_code               4028879