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_4028878
_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            'C31 H29 Cl3 F6 N4 O2'
_chemical_formula_weight         709.93
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5447(4)
_cell_length_b                   14.4270(5)
_cell_length_c                   19.4717(7)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.79
_cell_measurement_theta_min      3.93
_cell_volume                     3243.1(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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54959
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_correction_T_min  0.8602
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       needle
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+4.8210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                7233
_reflns_number_total             8462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo402277p_si_002_1.cif
_cod_data_source_block           C31H29Cl2F6N4O2
_cod_database_code               4028878