Twinned low-temperature structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate
Lutz, Martin; Acta Crystallographica Section C 66 (2010) m330–m335; doi:10.1107/S0108270110041466

data_2017836
_publ_section_title
;
 Twinned low-temperature structures of tris(ethylenediamine)zinc(II)
 sulfate and tris(ethylenediamine)copper(II) sulfate
;
_journal_coeditor_code           GG3243
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m330
_journal_page_last               m335
_journal_paper_doi               10.1107/S0108270110041466
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu (C2 H8 N2)3]2+, S O4 2-'
_chemical_formula_moiety         'C6 H24 Cu N6, O4 S'
_chemical_formula_sum            'C6 H24 Cu N6 O4 S'
_chemical_formula_weight         339.91
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1 (-x,-1/2*y+1/2*z,1/2*y+1/2*z)'
_symmetry_space_group_name_H-M   'A -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.582(3)
_cell_angle_beta                 90.296(5)
_cell_angle_gamma                119.845(4)
_cell_formula_units_Z            8
_cell_length_a                   8.8749(7)
_cell_length_b                   17.6358(11)
_cell_length_c                   19.1559(11)
_cell_measurement_reflns_used    5801
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.45
_cell_volume                     2600.5(3)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
EVAL14 (Duisenberg <i>et al.</i>, 2003), TWINABS (Sheldrick,
2008<i>a</i>)
;
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'manual edit of SHELXL cif file'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18964
_diffrn_reflns_theta_full        27.77
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.629
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0334P)^2^+3.8394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                4478
_reflns_number_total             5825
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3243.cif
_cod_data_source_block           II
_cod_original_sg_symbol_Hall     '-A 1'
_cod_database_code               2017836
_cod_database_fobs_code          2017836