Crystallisation, thermal analysis and acetal protection activity of new layered Zn(ii) hybrid polymorphs
Saïd, Salem; Naïli, Houcine; Bataille, Thierry; Herrera, Raquel P.; CrystEngComm 18 (2016) 5365–; doi:10.1039/C6CE00486E

data_7226167
_publ_section_title
;
 Crystallisation, thermal analysis and acetal protection activity of new
 layered Zn(ii) hybrid polymorphs
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5365
_journal_paper_doi               10.1039/C6CE00486E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '2(O4 S), 2(C6 H9 N2), H12 O6 Zn, 2(H2 O)'
_chemical_formula_sum            'C12 H34 N4 O16 S2 Zn'
_chemical_formula_weight         619.92
_chemical_name_systematic
;
 bis(2-amino-6-methylpyridinium) hexaaquazinc(II) disulfate dihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc13wg1h
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-27 deposited with the CCDC.
2016-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                80.60(3)
_cell_angle_beta                 83.38(3)
_cell_angle_gamma                89.56(3)
_cell_formula_units_Z            3
_cell_length_a                   7.3453(18)
_cell_length_b                   12.594(4)
_cell_length_c                   20.074(6)
_cell_measurement_reflns_used    8392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     1819.7(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type
;
Kuma KM-4-CCD\k-geometry 
;
_diffrn_measurement_method       'omega scan'
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14566
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.8733
_exptl_absorpt_correction_T_min  0.6655
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0650P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                6332
_reflns_number_total             8053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00486e3.cif
_cod_data_source_block           saleznra
_cod_database_code               7226167