Temperature-dependent analysis of thermal motion, disorder and structures of tris(ethylenediamine)zinc(II) sulfate and tris(ethylenediamine)copper(II) sulfate
Smeets, Stef; Parois, Pascal; Bürgi, Hans-Beat; Lutz, Martin; Acta Crystallographica Section B 67 (2011) 53–62; doi:10.1107/S0108768110054571

data_2104888
_publ_section_title
;
 Temperature-dependent analysis of thermal motion, disorder and
 structures of tris(ethylenediamine)zinc(II) sulfate and
 tris(ethylenediamine)copper(II) sulfate
;
_journal_coeditor_code           BK5101
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              53
_journal_page_last               62
_journal_paper_doi               10.1107/S0108768110054571
_journal_volume                  67
_journal_year                    2011
_chemical_formula_moiety         'C6 H24 Cu N6, O4 S'
_chemical_formula_sum            'C6 H24 Cu N6 O4 S'
_chemical_formula_weight         339.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   difmap
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.95130(10)
_cell_length_b                   8.95130(10)
_cell_length_c                   9.58760(10)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      2.12
_cell_volume                     665.293(13)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'EVAL15 (Schreurs et al., 2010), SADABS-2008/1 (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008a)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0103
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9736
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  0.9366
_exptl_absorpt_correction_T_min  0.5781
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'SADABS-2008/1 (Sheldrick, 2008b)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         687
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0315P)^2^+0.2737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                642
_reflns_number_total             687
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bk5101.cif
_cod_data_source_block           2c
_cod_original_cell_volume        665.293(16)
_cod_database_code               2104888
_cod_database_fobs_code          2104888