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_7226166
_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(C6 H9 N2), H12 O6 Zn, 2(O4 S), 2(H2 O)'
_chemical_formula_sum            'C12 H34 N4 O16 S2 Zn'
_chemical_formula_weight         619.94
_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/cc13wg0g
_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                106.77(4)
_cell_angle_beta                 104.90(4)
_cell_angle_gamma                98.84(4)
_cell_formula_units_Z            2
_cell_length_a                   7.3614(18)
_cell_length_b                   13.234(4)
_cell_length_c                   13.939(4)
_cell_measurement_reflns_used    5827
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     1217.8(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_device_type
;
'Xcalibur, Ruby' 
;
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9665
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   analytical
_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)
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    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0290P)^2^+0.6760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                5599
_reflns_number_total             7447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00486e3.cif
_cod_data_source_block           saleznba
_cod_original_cell_volume        1217.8(6)
_cod_original_formula_sum        'C12 H34 N4 O16 S2 Zn1'
_cod_database_code               7226166