Remarkable structural similarities between organic co-crystals and a metal–organic coordination network—insights into hydrogen bonded aliphatic ammonium chlorides
Baisch, Ulrich; Rubini, Katia; Braga, Dario; CrystEngComm 10 (2008) 1939–; doi:10.1039/b812892h

data_7202447
_publ_section_title
;
 Remarkable structural similarities between organic co-crystals and a
 metal--organic coordination network---insights into hydrogen bonded
 aliphatic ammonium chlorides
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1939
_journal_paper_doi               10.1039/b812892h
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C4 H12 N2, 0.5(H2 O), 2(Cl)'
_chemical_formula_sum            'C4 H13 Cl2 N2 O0.5'
_chemical_formula_weight         168.06
_chemical_name_common
;
dipiperazinium tetrachloride monohydrate
;
_chemical_name_systematic
;
dipiperazinium tetrachloride monohydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            8
_cell_length_a                   11.6011(11)
_cell_length_b                   9.6530(8)
_cell_length_c                   13.9669(12)
_cell_measurement_reflns_used    1765
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.8855
_cell_measurement_theta_min      2.5447
_cell_volume                     1564.1(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details
;
1 omega -41.00 53.80 1.2000 130.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -17.4392 45.0000 30.0000 0.0000 0.0000 79

2 omega -88.00 -35.20 1.2000 130.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -17.4392 -77.0000 270.0000 0.0000 0.0000 44

3 omega 11.00 42.20 1.2000 130.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 19.1580 -45.0000 30.0000 0.0000 0.0000 26

;
_diffrn_measurement_device       '95mm CCD camera (sapphire) on \k-goniostat'
_diffrn_measurement_device_type  xcalibur
_diffrn_measurement_method       'omega scan'
_diffrn_orient_matrix_UB_11      -0.0230008026
_diffrn_orient_matrix_UB_12      0.0263551432
_diffrn_orient_matrix_UB_13      -0.0428590105
_diffrn_orient_matrix_UB_21      -0.0202155303
_diffrn_orient_matrix_UB_22      -0.0546054986
_diffrn_orient_matrix_UB_23      -0.0179236353
_diffrn_orient_matrix_UB_31      -0.0662360849
_diffrn_orient_matrix_UB_32      0.0075368397
_diffrn_orient_matrix_UB_33      0.0202805561
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5299
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.3508
_exptl_crystal_size_mid          0.0787
_exptl_crystal_size_min          0.0329
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                1160
_reflns_number_total             1916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812892h.txt
_cod_data_source_block           ub043n_2
_cod_depositor_comments
;

2019-01-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C4 H12 N2), H2 O, 4(Cl)'
_cod_original_formula_sum        'C8 H26 Cl4 N4 O'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     336.13
_cod_database_code               7202447