#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/90/2239006.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_2239006
loop_
_publ_author_name
'Corfield, Peter W. R.'
'Michalski, Joseph F.'
_publ_section_title
;
 μ-Cyanido-κ²C:N-dicyanido-κ²C-bis(N-ethylethylenediamine-κ²N,N')copper(II)copper(I)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m76
_journal_page_last               m77
_journal_paper_doi               10.1107/S160053681400172X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Cu2 (C N)3 (C4 H12 N2)2]'
_chemical_formula_moiety         'C11 H24 Cu2 N7'
_chemical_formula_sum            'C11 H24 Cu2 N7'
_chemical_formula_weight         381.45
_chemical_name_systematic
;
μ-Cyanido-κ²C:N-dicyanido-κ²C-bis(N-ethylethylenediamine-κ²N,N')copper(II)copper(I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4250(10)
_cell_length_b                   9.679(2)
_cell_length_c                   15.205(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      19.07
_cell_measurement_theta_min      4.98
_cell_volume                     1680.8(5)
_computing_cell_refinement       'CAD-4 Software (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1994)'
_computing_data_reduction
;
data reduction followed procedures in Corfield et al. (1973);
data were averaged with a local version of SORTAV (Blessing, 1989)
;
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'θ/2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3737
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        2.3(6)
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.532
_exptl_absorpt_correction_T_max  0.5868
_exptl_absorpt_correction_T_min  0.5285
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Busing & Levy, 1957)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      1.497(2)
_exptl_crystal_density_method
;
Flotation in 1,2-dibromopropane/toluene mixtures.
Four independent determinations were made.
The observed density measurements were systematically 0.7% low, perhaps
due to the presence of occlusions in crystals that were large enough to use
for density measurements.
;
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.253
_refine_ls_extinction_coef       0.0078(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0199
_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/[σ²(Fo²)+(0.0000P)²+0.2500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                1674
_reflns_number_total             1835
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh5680sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2239006
_cod_database_fobs_code          2239006
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.5000 -0.29790(3) 0.2500 0.04340(12) Uani d S 1 2 . .
Cu Cu2 0.5000 0.24064(2) 0.2500 0.03031(11) Uani d S 1 2 . .
C C1 0.5000 -0.0984(3) 0.2500 0.0443(5) Uani d S 1 2 . .
N N1 0.5000 0.0193(2) 0.2500 0.0501(5) Uani d S 1 2 . .
C C2 0.39932(15) -0.40213(16) 0.32653(12) 0.0440(4) Uani d . 1 1 . .
N N2 0.34282(16) -0.46675(16) 0.37112(13) 0.0575(5) Uani d . 1 1 . .
N N3 0.67206(12) 0.29094(15) 0.27009(10) 0.0403(3) Uani d . 1 1 . .
H H3A 0.7170 0.2149 0.2662 0.048 Uiso calc R 1 1 A 1
H H3B 0.697(2) 0.341(2) 0.2337(15) 0.061(7) Uiso d . 1 1 B 2
C C4 0.68534(15) 0.35226(19) 0.35844(12) 0.0473(4) Uani d . 1 1 . .
H H4A 0.6590 0.4475 0.3574 0.071 Uiso calc R 1 1 . .
H H4B 0.7669 0.3505 0.3778 0.071 Uiso calc R 1 1 . .
C C5 0.61299(16) 0.2693(2) 0.41977(11) 0.0472(4) Uani d . 1 1 . .
H H5A 0.6443 0.1765 0.4254 0.071 Uiso calc R 1 1 . .
H H5B 0.6142 0.3117 0.4776 0.071 Uiso calc R 1 1 . .
N N6 0.49168(12) 0.26432(15) 0.38337(9) 0.0364(3) Uani d . 1 1 . .
H H6 0.4663(16) 0.342(2) 0.3875(12) 0.037(5) Uiso d . 1 1 . .
C C7 0.41570(17) 0.1642(2) 0.42882(12) 0.0498(4) Uani d . 1 1 . .
H H7A 0.4491 0.0726 0.4232 0.075 Uiso calc R 1 1 . .
H H7B 0.3394 0.1633 0.3993 0.075 Uiso calc R 1 1 . .
C C8 0.3996(2) 0.1943(3) 0.52557(13) 0.0670(6) Uani d . 1 1 . .
H H8A 0.4727 0.1814 0.5571 0.101 Uiso calc R 1 1 . .
H H8B 0.3420 0.1326 0.5484 0.101 Uiso calc R 1 1 . .
H H8C 0.3738 0.2880 0.5325 0.101 Uiso calc R 1 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-1 3 -1
10 0 0
0 4 0
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_3
_geom_angle
C1 Cu1 C2 . 6_656 121.32(5)
C1 Cu1 C2 . . 121.32(5)
C2 Cu1 C2 6_656 . 117.35(9)
N3 Cu2 N3 . 6_656 152.39(8)
N3 Cu2 N6 . . 83.96(6)
N3 Cu2 N6 6_656 . 92.97(6)
N3 Cu2 N6 . 6_656 92.97(6)
N3 Cu2 N6 6_656 6_656 83.96(6)
N6 Cu2 N6 . 6_656 167.13(8)
N3 Cu2 N1 . . 103.81(4)
N3 Cu2 N1 6_656 . 103.81(4)
N6 Cu2 N1 . . 96.43(4)
N6 Cu2 N1 6_656 . 96.43(4)
N1 C1 Cu1 . . 180.0
C1 N1 Cu2 . . 180.0
N2 C2 Cu1 . . 177.74(15)
C4 N3 Cu2 . . 107.96(10)
C4 N3 H3A . . 110.1
Cu2 N3 H3A . . 110.1
C4 N3 H3B . . 111.2(17)
Cu2 N3 H3B . . 114.1(18)
H3A N3 H3B . . 103.4
N3 C4 C5 . . 107.87(14)
N3 C4 H4A . . 110.1
C5 C4 H4A . . 110.1
N3 C4 H4B . . 110.1
C5 C4 H4B . . 110.1
H4A C4 H4B . . 108.4
N6 C5 C4 . . 108.17(14)
N6 C5 H5A . . 110.1
C4 C5 H5A . . 110.1
N6 C5 H5B . . 110.1
C4 C5 H5B . . 110.1
H5A C5 H5B . . 108.4
C5 N6 C7 . . 113.62(14)
C5 N6 Cu2 . . 107.86(10)
C7 N6 Cu2 . . 115.57(11)
C5 N6 H6 . . 106.0(13)
C7 N6 H6 . . 110.8(13)
Cu2 N6 H6 . . 102.0(13)
N6 C7 C8 . . 114.45(17)
N6 C7 H7A . . 108.6
C8 C7 H7A . . 108.6
N6 C7 H7B . . 108.6
C8 C7 H7B . . 108.6
H7A C7 H7B . . 107.6
C7 C8 H8A . . 109.5
C7 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
C7 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 C1 . 1.931(3) y
Cu1 C2 6_656 1.9406(18) ?
Cu1 C2 . 1.9406(18) y
Cu2 N3 . 2.0403(14) y
Cu2 N3 6_656 2.0403(14) ?
Cu2 N6 . 2.0456(14) y
Cu2 N6 6_656 2.0456(14) ?
Cu2 N1 . 2.142(2) y
C1 N1 . 1.139(4) y
C2 N2 . 1.136(2) y
N3 C4 . 1.473(2) ?
N3 H3A . 0.9000 ?
N3 H3B . 0.79(2) ?
C4 C5 . 1.496(3) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 N6 . 1.479(2) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
N6 C7 . 1.484(2) ?
N6 H6 . 0.81(2) ?
C7 C8 . 1.516(3) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N3 H3B N2 6_666 0.79(2) 2.49(2) 3.181(2) 147(2)
N6 H6 N2 1_565 0.81(2) 2.34(2) 3.112(2) 160.9(17)
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
N3 C4 C5 N6 -54.69(18)
C5 N6 C7 C8 61.5(2)
