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_7245706
_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_formula_sum            'C30 H32 N2'
_chemical_formula_weight         420.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-09-07 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.649(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   39.0954(15)
_cell_length_b                   12.9175(6)
_cell_length_c                   20.0670(6)
_cell_measurement_reflns_used    4895
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      73.9170
_cell_measurement_theta_min      3.5890
_cell_volume                     10113.6(7)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20091
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.082
_diffrn_reflns_theta_min         3.604
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.161
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.00017(3)
_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   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1121P)^2^+1.6575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1993
_refine_ls_wR_factor_ref         0.2334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6571
_reflns_number_total             9990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01174c2.cif
_cod_data_source_block           kdm1454
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7245706
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-4
_shelx_res_checksum              29104
_shelx_hkl_checksum              38954