The weakly coordinating perchlorate group in bis(<i>N</i>,<i>N</i>'-dimethylethylenediamine-κ^2^<i>N</i>,<i>N</i>')bis(perchlorato-κ<i>O</i>)copper(II) studied at 100, 250 and 400K
Schnitzler, Silvia; Şerb, Mihaela-Diana; Englert, Ulli; Acta Crystallographica Section C 68 (2012) m251–m254; doi:10.1107/S0108270112033318

data_2018663
_publ_section_title
;
 The weakly coordinating perchlorate group in
 bis(<i>N</i>,<i>N</i>'-dimethylethylenediamine-\k^2^<i>N</i>,<i>N</i>')bis(perchlorato-\k<i>O</i>)copper(II)
 studied at 100, 250 and 400K
;
_journal_coeditor_code           SK3443
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m251
_journal_page_last               m254
_journal_paper_doi               10.1107/S0108270112033318
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu (Cl O4)2 (C4 H12 N2)2]'
_chemical_formula_moiety         'C8 H24 Cl2 Cu N4 O8'
_chemical_formula_sum            'C8 H24 Cl2 Cu N4 O8'
_chemical_formula_weight         438.75
_chemical_name_systematic
;
bis(<i>N</i>,<i>N</i>'-dimethylethylenediamine-
\k^2^<i>N</i>,<i>N</i>')bis(perchlorato-\k<i>O</i>)copper(II)]
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.866(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.731(3)
_cell_length_b                   13.824(5)
_cell_length_c                   15.314(6)
_cell_measurement_reflns_used    1270
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.67
_cell_volume                     1841.7(12)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      400(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type
'Bruker D8 goniometer with a SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9966
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.373
_refine_ls_abs_structure_details 'Flack (1983), with 1702 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3479
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                2156
_reflns_number_total             3479
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3443.cif
_cod_data_source_block           Ic
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2018663
_cod_database_fobs_code          2018663