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_2018662
_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                 95.533(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5966(14)
_cell_length_b                   13.655(2)
_cell_length_c                   14.966(3)
_cell_measurement_reflns_used    1054
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      17.40
_cell_measurement_theta_min      2.73
_cell_volume                     1748.6(5)
_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      250(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0819
_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       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10331
_diffrn_reflns_theta_full        26.52
_diffrn_reflns_theta_max         26.52
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.597
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.289
_refine_ls_abs_structure_details 'Flack (1983), with 1793 Friedel pairs'
_refine_ls_abs_structure_Flack   0.011(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3607
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                2853
_reflns_number_total             3607
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3443.cif
_cod_data_source_block           Ib
_cod_original_cell_volume        1748.5(5)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2018662
_cod_database_fobs_code          2018662