Structural aspects of intermolecular interactions in the solid state of 1,4-dibenzylpiperazines bearing nitrile or amidine groups
Rezler, Mateusz; Żołek, Teresa; Wolska, Irena; Maciejewska, Dorota; Acta Crystallographica Section B 70 (2014) 820–827; doi:10.1107/S2052520614013754

data_2105962
_publ_section_title
;
 Structural aspects of intermolecular interactions in the solid state of
 1,4-dibenzylpiperazines bearing nitrile or amidine groups
;
_journal_coeditor_code           BM5065
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              820
_journal_page_last               827
_journal_paper_doi               10.1107/S2052520614013754
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C20 H30 N6, 4(Cl), 4(H2 O)'
_chemical_formula_sum            'C20 H38 Cl4 N6 O4'
_chemical_formula_weight         568.36
_chemical_name_systematic
;
1,4-bis(4-amidinobenzyl)piperazine tetrahydrochloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.274(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1121(2)
_cell_length_b                   12.8231(3)
_cell_length_c                   18.3831(4)
_cell_measurement_reflns_used    1496
_cell_measurement_temperature    130.0(10)
_cell_measurement_theta_max      61.5448
_cell_measurement_theta_min      2.4316
_cell_volume                     1421.96(7)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2012)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2012)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2012)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130.0(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6224
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         75.40
_diffrn_reflns_theta_min         4.22
_exptl_absorpt_coefficient_mu    4.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
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_refine_diff_density_min         -0.211
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         2866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0403P)^2^+0.5773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                2771
_reflns_number_total             2866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm5065sup1.cif
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_cod_depositor_comments
'Adding full bibliography for 2105961--2105962.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               2105962