Solid-state stability of Z’ < 1 and Z’ = 2 polymorphs of N,N,N’,N’-tetrabenzylethylenediamine: a combined experimental and theoretical study.
Wang, Zhen; Cui, Xiaoxiao; Famulari, Antonino; Marti-Rujas, Javier; Kariuki, Benson; Guo, Fang; CrystEngComm  (2022) –; doi:10.1039/D2CE01174C

data_7245707
_publ_section_title
;
 Solid-state stability of Z&#x2019; &lt; 1 and Z&#x2019; = 2 polymorphs of
 N,N,N&#x2019;,N&#x2019;-tetrabenzylethylenediamine: a combined
 experimental and theoretical study.
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01174C
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_sum            'C15 H16 N'
_chemical_formula_weight         210.29
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_audit_update_record
;
2021-09-15 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                76.992(8)
_cell_angle_beta                 86.676(7)
_cell_angle_gamma                79.275(8)
_cell_formula_units_Z            2
_cell_length_a                   6.356(4)
_cell_length_b                   9.042(6)
_cell_length_c                   11.117(7)
_cell_measurement_reflns_used    1152
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.66
_cell_volume                     611.5(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3282
_diffrn_reflns_theta_full        12.50
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 240
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             226
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.086(13)
_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   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1497
_reflns_number_gt                1657
_reflns_number_total             2594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2ce01174c2.cif
_cod_data_source_block           gf2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7245707