Inorganic layered structures in hybrid double sulfates: related phases and thermal reactivity
Kammoun, Omar; Rekik, Walid; Naïli, Houcine; Bataille, Thierry; New J. Chem. 39 (2015) 2682–; doi:10.1039/C4NJ02195A

data_7054639
_publ_section_title
;
 Inorganic layered structures in hybrid double sulfates: related phases
 and thermal reactivity
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              2682
_journal_paper_doi               10.1039/C4NJ02195A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         '2(C7 H7 N2), Cu H12 O6, 2(O4 S), 4(H2 O)'
_chemical_formula_sum            'C14 H34 Cu N4 O18 S2'
_chemical_formula_weight         674.11
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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/cc13pwl8
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-13 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                85.4290(10)
_cell_angle_beta                 81.4370(10)
_cell_angle_gamma                85.4360(10)
_cell_formula_units_Z            1
_cell_length_a                   6.82920(10)
_cell_length_b                   8.1314(2)
_cell_length_c                   12.3445(3)
_cell_measurement_reflns_used    2477
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.032
_cell_measurement_theta_min      2.910
_cell_volume                     674.11(3)
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8898
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.9914
_exptl_absorpt_correction_T_min  0.8503
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(c.f. r.h. blessing, acta cryst. (1995), a51, 33-38) 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Polyhedral
_exptl_crystal_F_000             351
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.542
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.093(10)
_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   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0559P)^2^+0.5805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                4067
_reflns_number_total             4622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj02195a2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7054638--7054641.cif.'
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054639