#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/55/2235564.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2235564
loop_
_publ_author_name
'Corfield, Peter W. R.'
'Yang, Sylvia C.'
_publ_section_title
;
 catena-Poly[[[(diethylenetriamine-κ³N,N',N'')copper(II)]-μ-cyanido-κ²C:N]
 perchlorate]
;
_journal_coeditor_code           PK2408
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m872
_journal_page_last               m873
_journal_paper_doi               10.1107/S1600536812023987
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu (C N) (C4 H13 N3)] Cl O4'
_chemical_formula_moiety         'C5 H13 Cu N4 +, Cl O4 -'
_chemical_formula_structural     '(Cu(C4 H13 N3) (C N) ) (Cl O4)'
_chemical_formula_sum            'C5 H13 Cl Cu N4 O4'
_chemical_formula_weight         292.18
_chemical_melting_point          471(2)
_chemical_name_systematic
;
catena-Poly[[[(diethylenetriamine-
κ³N,N',N'')copper(II)]-μ-cyanido-
κ²C:N] perchlorate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   vecmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.109(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7767(8)
_cell_length_b                   21.5081(16)
_cell_length_c                   8.3635(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      52
_cell_measurement_theta_min      4
_cell_volume                     1075.2(2)
_computing_cell_refinement       'locally modified program (Corfield, 1972)'
_computing_data_collection       'locally modified program (Corfield, 1972)'
_computing_data_reduction
;
cell refinements and data reduction follow procedures in (Corfield et
al.,
1967) and (Corfield & Shore, 1973). Standard deviations of
intensities include
an ignorance factor (Busing & Levy, 1957b) set here to 0.06
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
;
local superposition program (Corfield, 1972)
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Picker four-circle'
_diffrn_measurement_method       'θ/2θ scans'
_diffrn_radiation_monochromator  'oriented graphite 200 reflection'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3044
_diffrn_reflns_theta_full        63.32
_diffrn_reflns_theta_max         63.32
_diffrn_reflns_theta_min         4.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    5.287
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Busing & Levy, 1957a)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      1.805
_exptl_crystal_density_method    ' flotation in chloroform/bromoform mixtures'
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.354
_refine_ls_extinction_coef       0.0010(2)
_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   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0306
_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)+(0.0100P)²+1.1400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                1625
_reflns_number_total             1752
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2408.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2235564
_cod_database_fobs_code          2235564
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, 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 Cu 0.15547(7) 0.322023(18) 0.63505(5) 0.03271(18) Uani d . 1 1 . .
N N1 -0.0930(4) 0.38484(12) 0.5101(3) 0.0426(6) Uani d . 1 1 . .
H H1A -0.0788 0.4034 0.4197 0.051 Uiso calc R 1 1 . .
H H1B -0.2264 0.3655 0.4620 0.051 Uiso calc R 1 1 . .
C C2 -0.0818(6) 0.43180(15) 0.6424(5) 0.0499(8) Uani d . 1 1 . .
H H2A -0.1495 0.4157 0.7135 0.075 Uiso calc R 1 1 . .
H H2B -0.1626 0.4689 0.5799 0.075 Uiso calc R 1 1 . .
C C3 0.1595(5) 0.44708(14) 0.7639(4) 0.0433(7) Uani d . 1 1 . .
H H3A 0.2220 0.4689 0.6965 0.065 Uiso calc R 1 1 . .
H H3B 0.1743 0.4734 0.8632 0.065 Uiso calc R 1 1 . .
N N4 0.2770(4) 0.38751(10) 0.8338(3) 0.0321(5) Uani d . 1 1 . .
H H4 0.2433 0.3746 0.9217 0.038 Uiso calc R 1 1 . .
C C5 0.5219(5) 0.38908(15) 0.9155(4) 0.0410(7) Uani d . 1 1 . .
H H5A 0.5851 0.4108 1.0307 0.061 Uiso calc R 1 1 . .
H H5B 0.5674 0.4104 0.8360 0.061 Uiso calc R 1 1 . .
C C6 0.6010(6) 0.32285(15) 0.9427(5) 0.0481(8) Uani d . 1 1 . .
H H6A 0.7601 0.3214 0.9809 0.072 Uiso calc R 1 1 . .
H H6B 0.5750 0.3034 1.0358 0.072 Uiso calc R 1 1 . .
N N7 0.4756(4) 0.28942(12) 0.7688(4) 0.0430(6) Uani d . 1 1 . .
H H7A 0.4741 0.2484 0.7900 0.052 Uiso calc R 1 1 . .
H H7B 0.5436 0.2949 0.6997 0.052 Uiso calc R 1 1 . .
C C8 0.0609(5) 0.26492(13) 0.4243(4) 0.0344(6) Uani d . 1 1 . .
N N8 0.0196(4) 0.23248(12) 0.3050(3) 0.0428(6) Uani d . 1 1 . .
Cl Cl 0.30284(12) 0.40553(3) 0.28806(10) 0.0381(2) Uani d . 1 1 . .
O O2 0.4055(5) 0.45800(12) 0.2534(4) 0.0653(7) Uani d . 1 1 A .
O O1 0.0662(8) 0.4083(3) 0.1838(8) 0.0782(19) Uani d P 0.70 1 A 1
O O3 0.3915(7) 0.35240(17) 0.2420(6) 0.0528(10) Uani d P 0.70 1 A 1
O O4 0.3631(8) 0.4055(2) 0.4760(6) 0.0593(12) Uani d P 0.70 1 A 1
O O1' 0.109(3) 0.3883(9) 0.125(3) 0.069(5) Uiso d P 0.18 1 A 1
O O3' 0.440(3) 0.3468(7) 0.349(2) 0.053(3) Uiso d P 0.18 1 A 1
O O4' 0.238(3) 0.4161(8) 0.419(2) 0.056(4) Uiso d P 0.18 1 A 1
O O1'' 0.077(8) 0.421(2) 0.243(5) 0.069(5) Uiso d P 0.12 1 A 2
O O3'' 0.286(4) 0.3518(13) 0.183(4) 0.053(3) Uiso d P 0.12 1 A 2
O O4'' 0.413(5) 0.3815(12) 0.474(4) 0.056(4) Uiso d P 0.12 1 A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
C8 Cu N1 . 96.45(11)
C8 Cu N4 . 171.38(11)
N1 Cu N4 . 82.98(10)
C8 Cu N7 . 95.09(11)
N1 Cu N7 . 157.48(11)
N4 Cu N7 . 82.73(10)
C8 Cu N8 2 100.04(10)
N1 Cu N8 2 100.27(11)
N4 Cu N8 2 88.51(9)
N7 Cu N8 2 96.66(10)
C2 N1 Cu . 109.50(19)
C2 N1 H1A . 109.8
Cu N1 H1A . 109.8
C2 N1 H1B . 109.8
Cu N1 H1B . 109.8
H1A N1 H1B . 108.2
N1 C2 C3 . 108.2(3)
N1 C2 H2A . 110.1
C3 C2 H2A . 110.1
N1 C2 H2B . 110.1
C3 C2 H2B . 110.1
H2A C2 H2B . 108.4
N4 C3 C2 . 106.9(2)
N4 C3 H3A . 110.3
C2 C3 H3A . 110.3
N4 C3 H3B . 110.3
C2 C3 H3B . 110.3
H3A C3 H3B . 108.6
C5 N4 C3 . 116.4(2)
C5 N4 Cu . 109.27(17)
C3 N4 Cu . 110.01(18)
C5 N4 H4 . 106.9
C3 N4 H4 . 106.9
Cu N4 H4 . 106.9
N4 C5 C6 . 107.1(2)
N4 C5 H5A . 110.3
C6 C5 H5A . 110.3
N4 C5 H5B . 110.3
C6 C5 H5B . 110.3
H5A C5 H5B . 108.6
N7 C6 C5 . 108.3(3)
N7 C6 H6A . 110.0
C5 C6 H6A . 110.0
N7 C6 H6B . 110.0
C5 C6 H6B . 110.0
H6A C6 H6B . 108.4
C6 N7 Cu . 109.98(19)
C6 N7 H7A . 109.7
Cu N7 H7A . 109.7
C6 N7 H7B . 109.7
Cu N7 H7B . 109.7
H7A N7 H7B . 108.2
N8 C8 Cu . 175.9(3)
C8 N8 Cu 2_554 146.5(2)
O1 Cl O2 . 111.1(3)
O1 Cl O3 . 111.4(3)
O1 Cl O4 . 109.3(3)
O2 Cl O3 . 105.7(2)
O2 Cl O4 . 108.1(2)
O3 Cl O4 . 111.1(3)
O1' Cl O2 . 109.3(8)
O1' Cl O3' . 104.4(10)
O1' Cl O4' . 107.9(11)
O2 Cl O3' . 116.7(6)
O2 Cl O4' . 113.6(7)
O3' Cl O4' . 104.3(9)
O1'' Cl O2 . 108.8(18)
O1'' Cl O3'' . 105.5(17)
O1'' Cl O4'' . 108(2)
O2 Cl O3'' . 114.8(11)
O2 Cl O4'' . 116.1(12)
O3'' Cl O4'' . 102.8(15)
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
Cu C8 . 1.990(3) y
Cu N1 . 2.023(2) y
Cu N4 . 2.034(2) y
Cu N7 . 2.040(3) y
Cu N8 2 2.340(3) y
N1 C2 . 1.474(4) ?
N1 H1A . 0.9000 ?
N1 H1B . 0.9000 ?
C2 C3 . 1.500(5) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 N4 . 1.476(4) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
N4 C5 . 1.467(4) ?
N4 H4 . 0.9100 ?
C5 C6 . 1.501(4) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 N7 . 1.480(4) ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
N7 H7A . 0.9000 ?
N7 H7B . 0.9000 ?
C8 N8 . 1.139(4) y
N8 Cu 2_554 2.340(3) ?
Cl O1 . 1.420(5) ?
Cl O2 . 1.425(2) ?
Cl O3 . 1.426(4) ?
Cl O4 . 1.426(4) ?
Cl O1' . 1.43(2) ?
Cl O3' . 1.507(15) ?
Cl O4' . 1.376(16) ?
Cl O1'' . 1.44(5) ?
Cl O3'' . 1.42(3) ?
Cl O4'' . 1.46(3) ?
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
N1 H1B O3 1_455 0.90 2.38 3.215(5) 153.8
N4 H4 O3 1_556 0.91 2.42 3.214(5) 145.3
N7 H7A O3 2 0.90 2.23 3.092(4) 160.5
N1 H1A O4' . 0.90 2.17 2.771(17) 123.8
N1 H1B O3' 1_455 0.90 2.04 2.913(15) 163.7
N4 H4 O1' 1_556 0.91 2.30 3.139(19) 153.9
N7 H7A O3' 2 0.90 2.14 3.040(16) 173.3
N1 H1A O1'' . 0.90 2.21 3.06(4) 155.6
N1 H1B O4'' 1_455 0.90 2.51 3.21(3) 135.2
N4 H4 O3'' 1_556 0.91 2.12 2.99(3) 159.7
N7 H7A O3'' 2 0.90 2.45 3.24(3) 147.4
N7 H7B O4'' . 0.90 2.50 3.04(3) 118.6
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
N1 C2 C3 N4 -51.9(3)
N4 C5 C6 N7 51.9(3)
