#------------------------------------------------------------------------------
#$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $
#$Revision: 14 $
#$URL: svn://www.crystallography.net/cod/cif/2/2203209.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2203209
loop_
_publ_author_name
'Akitsu, Takashiro'
'Einaga, Yasuaki'
_publ_section_title
;
Bis(N,N-dimethylethylenediamine-\k^2^N,N')bis(perchlorato-\kO)copper(II)
;
_journal_issue                 2
_journal_name_full             'Acta Crystallographica, Section E'
_journal_page_first            m234
_journal_page_last             m236
_journal_volume                60
_journal_year                  2004
_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       438.76
_chemical_melting_point        ?
_symmetry_cell_setting         triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha              111.01(6)
_cell_angle_beta               104.91(6)
_cell_angle_gamma              61.65(3)
_cell_formula_units_Z          1
_cell_length_a                 7.978(4)
_cell_length_b                 8.593(4)
_cell_length_c                 7.797(8)
_cell_measurement_reflns_used  17
_cell_measurement_temperature  297.2
_cell_measurement_theta_max    12.4
_cell_measurement_theta_min    11.2
_cell_volume                   436.7(6)
_computing_cell_refinement     'WinAFC Diffractmeter Control Software'
_computing_data_collection
'WinAFC Diffractmeter Control Software (Rigaku, 1999)'
_computing_data_reduction      'TEXSAN (Molecular Structure Corporation, 2001)'
_computing_molecular_graphics  'ORTEPII (Johnson, 1976)'
_computing_publication_material TEXSAN
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution  'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type 'Rigaku AFC-7R'
_diffrn_measurement_method     \w-2\q
_diffrn_radiation_type         'Mo K\a'
_diffrn_radiation_wavelength   0.7107
_diffrn_reflns_av_R_equivalents 0.061
_diffrn_reflns_limit_h_max     10
_diffrn_reflns_limit_h_min     -10
_diffrn_reflns_limit_k_max     10
_diffrn_reflns_limit_k_min     -11
_diffrn_reflns_limit_l_max     10
_diffrn_reflns_limit_l_min     -4
_diffrn_reflns_number          2269
_diffrn_reflns_theta_full      27.50
_diffrn_reflns_theta_max       27.50
_diffrn_reflns_theta_min       ?
_diffrn_standards_decay_%      2.45
_diffrn_standards_interval_count 150
_diffrn_standards_number       3
_exptl_absorpt_coefficient_mu  1.599
_exptl_absorpt_correction_T_max 0.726
_exptl_absorpt_correction_T_min 0.625
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ' (North et al., 1968)'
_exptl_crystal_colour          blue
_exptl_crystal_density_diffrn  1.668
_exptl_crystal_density_meas    ?
_exptl_crystal_density_method  'not measured'
_exptl_crystal_description     prismatic
_exptl_crystal_F_000           227.0
_exptl_crystal_size_max        0.300
_exptl_crystal_size_mid        0.300
_exptl_crystal_size_min        0.200
_exptl_crystal_size_rad        ?
_refine_diff_density_max       0.41
_refine_diff_density_min       -0.48
_refine_ls_extinction_coef     0.0234
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method   SHELXL97
_refine_ls_goodness_of_fit_ref 0.908
_refine_ls_hydrogen_treatment  noref
_refine_ls_number_parameters   107
_refine_ls_number_reflns       1894
_refine_ls_R_factor_gt         0.0310
_refine_ls_shift/su_max        0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0348P)^2^+0.3309P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme    calc
_refine_ls_wR_factor_ref       0.1133
_reflns_number_gt              1894
_reflns_number_total           2007
_reflns_threshold_expression   I>2\s(I)
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 1.0000 0.0000 1.0000 0.0299(2) Uani d S 1.00 . . Cu
Cl1 0.69554(8) -0.03463(9) 1.28417(8) 0.0424(2) Uani d . 1.00 . . Cl
O1 0.7340(4) -0.0038(4) 1.1324(3) 0.0659(6) Uani d . 1.00 . . O
O2 0.6051(5) -0.1540(5) 1.2124(5) 0.0950(10) Uani d . 1.00 . . O
O3 0.5763(4) 0.1339(4) 1.3993(4) 0.0830(8) Uani d . 1.00 . . O
O4 0.8734(4) -0.1147(5) 1.3878(4) 0.0970(10) Uani d . 1.00 . . O
N1 1.1934(3) -0.0955(3) 1.1993(3) 0.0373(4) Uani d . 1.00 . . N
N2 1.0633(3) -0.2773(3) 0.8601(3) 0.0371(4) Uani d . 1.00 . . N
C1 1.2861(4) -0.2994(4) 1.1424(4) 0.0486(6) Uani d . 1.00 . . C
C2 1.1470(4) -0.3695(3) 1.0107(4) 0.0442(6) Uani d . 1.00 . . C
C3 0.8964(5) -0.3159(4) 0.7599(4) 0.0555(7) Uani d . 1.00 . . C
C4 1.2046(5) -0.3542(4) 0.7260(4) 0.0546(7) Uani d . 1.00 . . C
H1 1.2883 -0.0499 1.2257 0.0442 Uiso calc . 1.00 . . H
H2 1.1323 -0.0530 1.3075 0.0442 Uiso calc . 1.00 . . H
H3 1.3973 -0.3415 1.0838 0.0566 Uiso calc . 1.00 . . H
H4 1.3246 -0.3431 1.2493 0.0566 Uiso calc . 1.00 . . H
H5 1.0477 -0.3452 1.0767 0.0522 Uiso calc . 1.00 . . H
H6 1.2121 -0.4993 0.9596 0.0522 Uiso calc . 1.00 . . H
H7 0.8030 -0.2693 0.8444 0.0656 Uiso calc . 1.00 . . H
H8 0.8381 -0.2571 0.6639 0.0656 Uiso calc . 1.00 . . H
H9 0.9347 -0.4446 0.7096 0.0656 Uiso calc . 1.00 . . H
H10 1.2456 -0.4834 0.6779 0.0649 Uiso calc . 1.00 . . H
H11 1.1498 -0.2984 0.6273 0.0649 Uiso calc . 1.00 . . H
H12 1.3141 -0.3297 0.7870 0.0649 Uiso calc . 1.00 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.0295(2) 0.0287(2) 0.0301(2) -0.0130(2) -0.00080(10) 0.00850(10)
Cl1 0.0358(3) 0.0563(4) 0.0394(4) -0.0226(3) 0.0034(3) 0.0142(3)
O1 0.0730(10) 0.079(2) 0.0610(10) -0.0350(10) 0.0200(10) 0.0230(10)
O2 0.103(2) 0.096(2) 0.118(3) -0.072(2) 0.017(2) 0.020(2)
O3 0.076(2) 0.077(2) 0.070(2) -0.0090(10) 0.0300(10) 0.0110(10)
O4 0.0520(10) 0.149(3) 0.0550(10) -0.011(2) -0.0030(10) 0.042(2)
N1 0.0350(10) 0.0375(10) 0.0340(9) -0.0143(8) -0.0031(8) 0.0102(8)
N2 0.0410(10) 0.0328(9) 0.0372(10) -0.0176(8) 0.0011(8) 0.0084(8)
C1 0.0470(10) 0.0370(10) 0.051(2) -0.0110(10) -0.0050(10) 0.0180(10)
C2 0.0500(10) 0.0340(10) 0.0500(10) -0.0170(10) 0.0010(10) 0.0160(10)
C3 0.061(2) 0.0490(10) 0.057(2) -0.0350(10) -0.0080(10) 0.0090(10)
C4 0.066(2) 0.0450(10) 0.050(2) -0.0190(10) 0.0210(10) 0.0050(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cu Cu 0.320 1.265
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cu1 N1 . . . 90.90(10) yes
O1 Cu1 N2 . . . 85.65(9) yes
N1 Cu1 N2 . . . 85.40(8) yes
O1 Cl1 O2 . . . 108.2(2) no
O1 Cl1 O3 . . . 110.5(2) no
O1 Cl1 O4 . . . 107.8(2) no
O2 Cl1 O3 . . . 110.1(2) no
O2 Cl1 O4 . . . 110.9(2) no
O3 Cl1 O4 . . . 109.2(2) no
Cu1 O1 Cl1 . . . 143.30(10) no
Cu1 N1 C1 . . . 110.80(10) no
Cu1 N1 H1 . . . 109.0 no
Cu1 N1 H2 . . . 109.2 no
C1 N1 H1 . . . 109.5 no
C1 N1 H2 . . . 109.4 no
H1 N1 H2 . . . 109.0 no
Cu1 N2 C2 . . . 103.50(10) no
Cu1 N2 C3 . . . 115.30(10) yes
Cu1 N2 C4 . . . 111.7(2) yes
C2 N2 C3 . . . 108.4(3) no
C2 N2 C4 . . . 110.3(2) no
C3 N2 C4 . . . 107.6(2) no
N1 C1 C2 . . . 109.2(2) no
N1 C1 H3 . . . 109.4 no
N1 C1 H4 . . . 109.3 no
C2 C1 H3 . . . 109.9 no
C2 C1 H4 . . . 110.4 no
H3 C1 H4 . . . 108.6 no
N2 C2 C1 . . . 110.2(3) no
N2 C2 H5 . . . 109.9 no
N2 C2 H6 . . . 109.8 no
C1 C2 H5 . . . 109.0 no
C1 C2 H6 . . . 109.2 no
H5 C2 H6 . . . 108.7 no
N2 C3 H7 . . . 109.4 no
N2 C3 H8 . . . 110.6 no
N2 C3 H9 . . . 110.4 no
H7 C3 H8 . . . 108.3 no
H7 C3 H9 . . . 108.4 no
H8 C3 H9 . . . 109.7 no
N2 C4 H10 . . . 110.3 no
N2 C4 H11 . . . 110.4 no
N2 C4 H12 . . . 109.5 no
H10 C4 H11 . . . 109.4 no
H10 C4 H12 . . . 108.7 no
H11 C4 H12 . . . 108.4 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O1 . . 2.605(4) yes
Cu1 N1 . . 1.987(2) yes
Cu1 N2 . . 2.098(2) yes
Cl1 O1 . . 1.433(4) yes
Cl1 O2 . . 1.404(4) yes
Cl1 O3 . . 1.416(3) yes
Cl1 O4 . . 1.421(3) yes
N1 C1 . . 1.482(3) yes
N1 H1 . . 0.955 no
N1 H2 . . 0.951 no
N2 C2 . . 1.487(4) yes
N2 C3 . . 1.480(4) yes
N2 C4 . . 1.485(4) yes
C1 C2 . . 1.501(4) yes
C1 H3 . . 0.955 no
C1 H4 . . 0.955 no
C2 H5 . . 0.955 no
C2 H6 . . 0.954 no
C3 H7 . . 0.964 no
C3 H8 . . 0.950 no
C3 H9 . . 0.948 no
C4 H10 . . 0.948 no
C4 H11 . . 0.952 no
C4 H12 . . 0.961 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H2 O1 . . . 0.95 3.01 3.300(4) 99 no
N1 H2 O4 . . . 0.95 2.62 3.348(5) 133 no
N1 H1 O2 . . 1_655 0.96 2.26 3.057(5) 140 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cu1 O1 Cl1 O2 . . . . -131.5(3) no
Cu1 O1 Cl1 O3 . . . . 107.9(3) no
Cu1 O1 Cl1 O4 . . . . -11.4(3) no
Cu1 N1 C1 C2 . . . . -29.8(3) no
Cu1 N2 C2 C1 . . . . -44.0(2) no
Cl1 O1 Cu1 N1 . . . . 6.1(3) no
Cl1 O1 Cu1 N2 . . . . 91.4(3) no
O1 Cu1 N1 C1 . . . . 89.8(2) no
O1 Cu1 N2 C2 . . . . -69.6(2) no
O1 Cu1 N2 C3 . . . . 48.6(2) no
O1 Cu1 N2 C4 . . . . 171.8(2) no
N1 Cu1 N2 C2 . . . . 21.6(2) no
N1 Cu1 N2 C3 . . . . 139.8(2) no
N1 Cu1 N2 C4 . . . . -96.9(2) no
N1 C1 C2 N2 . . . . 50.5(3) yes
N2 Cu1 N1 C1 . . . . 4.2(2) no
C1 C2 N2 C3 . . . . -166.9(2) no
C1 C2 N2 C4 . . . . 75.6(3) no