#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/27/2232769.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_2232769
loop_
_publ_author_name
'Oelkers, Benjamin'
'Stricker, Marion'
'Sundermeyer, Jörg'
_publ_section_title
;
 catena-Poly[[diacetonitrilecopper(I)]-μ-dicyanamido]
;
_journal_coeditor_code           HP2020
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1784
_journal_paper_doi               10.1107/S1600536811047052
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Cu (C2 N3) (C2 H3 N)2]'
_chemical_formula_moiety         'C6 H6 Cu N5'
_chemical_formula_sum            'C6 H6 Cu N5'
_chemical_formula_weight         211.71
_chemical_name_systematic
;
catena-Poly[[diacetonitrilecopper(I)]-μ-dicyanamido]
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.5222(5)
_cell_length_b                   10.5307(11)
_cell_length_c                   5.5378(4)
_cell_measurement_reflns_used    9024
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      1.93
_cell_volume                     438.67(6)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4132
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         3.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  0.7832
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.892
_refine_diff_density_min         -1.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0320
_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/[σ²(Fo²)+(0.0425P)²+0.0839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0660
_reflns_number_gt                510
_reflns_number_total             528
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL ms083 in P m m n
CELL  0.71073   7.5222  10.5307   5.5378   90.000   90.000   90.000
ZERR     2.00   0.0005   0.0011   0.0004    0.000    0.000    0.000
LATT   1
SYMM  1/2 - X, 1/2 - Y,   Z
SYMM  1/2 + X, - Y, - Z
SYMM  - X, 1/2 + Y, - Z
SFAC  C    H    N    CU
UNIT  12   12   10   2
MERG   2
FMAP   2
PLAN   25
ACTA    50.00
BOND   $H
CONF
L.S.   4
TEMP  -173.00
WGHT    0.042500    0.083900
FVAR       1.31169
CU1   4    0.750000    0.750000    0.377472    10.25000    0.02419    0.02519 =
         0.02242    0.00000    0.00000    0.00000
N1    3    0.250000    0.750000    0.801736    10.25000    0.02330    0.03422 =
         0.02245    0.00000    0.00000    0.00000
N2    3    0.534617    0.750000    0.581043    10.50000    0.02414    0.03119 =
         0.02560    0.00000   -0.00215    0.00000
N3    3    0.750000    0.895835    0.140241    10.50000    0.03484    0.02675 =
         0.02808    0.00068    0.00000    0.00000
C1    1    0.398685    0.750000    0.677904    10.50000    0.02585    0.02138 =
         0.02046    0.00000   -0.00441    0.00000
C2    1    0.750000    1.039748   -0.241293    10.50000    0.04627    0.02462 =
         0.02454    0.00280    0.00000    0.00000
AFIX   3
H2A   2    0.750000    0.986289   -0.386146    10.50000   -1.50000
H2B   2    0.856178    1.093673   -0.240664    11.00000   -1.50000
AFIX   0
C3    1    0.750000    0.959471   -0.026982    10.50000    0.03069    0.02350 =
         0.02606   -0.00140    0.00000    0.00000
HKLF    4
REM  ms083 in P m m n
REM R1 =  0.0320 for    510 Fo > 4sig(Fo)  and  0.0326 for all    528 data
REM     39 parameters refined using      0 restraints
END
WGHT      0.0425      0.0839
REM Highest difference peak  0.892,  deepest hole -1.050,  1-sigma level  0.157
Q1    1   0.7500  0.7500  0.5948  10.25000  0.05    0.89
Q2    1   0.7500  0.7500  0.1426  10.25000  0.05    0.68
Q3    1   0.7500  0.9003 -0.1075  10.50000  0.05    0.54
Q4    1   0.6963  0.8692  0.3410  11.00000  0.05    0.43
Q5    1   0.4982  0.7500  0.3868  10.50000  0.05    0.43
Q6    1   0.5194  0.7500  0.8413  10.50000  0.05    0.35
Q7    1   0.7500  0.9774 -0.1243  10.50000  0.05    0.32
Q8    1   0.8688  0.6775  0.2600  11.00000  0.05    0.29
Q9    1   0.9611  1.1320 -0.0771  11.00000  0.05    0.28
Q10   1   0.4670  0.8717  0.6627  11.00000  0.05    0.27
Q11   1   0.5564  0.8768  0.6267  11.00000  0.05    0.21
Q12   1   0.5891  0.9999 -0.4718  11.00000  0.05    0.21
Q13   1   0.5339  0.9256 -0.3018  11.00000  0.05    0.20
Q14   1   0.2500  0.6683  0.9217  10.50000  0.05    0.19
Q15   1   0.7500  1.1094 -0.2612  10.50000  0.05    0.16
Q16   1   0.8962  1.0339 -0.2915  11.00000  0.05    0.15
Q17   1   0.8511  1.2500 -0.2222  10.50000  0.05    0.14
Q18   1   0.7500  1.2500 -0.2652  10.25000  0.05    0.14
Q19   1   1.0221  0.9727 -0.1814  11.00000  0.05    0.12
Q20   1   0.6505  1.0436  0.1469  11.00000  0.05    0.11
Q21   1   0.5887  0.9965  0.1475  11.00000  0.05    0.11
Q22   1   0.6272  1.0163  0.1767  11.00000  0.05    0.11
Q23   1   0.2500  0.7500  0.5266  10.25000  0.05    0.09
Q24   1   0.8628  1.1007 -0.3768  11.00000  0.05    0.04
Q25   1   0.8886  0.9889 -0.1473  11.00000  0.05    0.01
;
_cod_data_source_file            hp2020.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               2232769
_cod_database_fobs_code          2232769
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'
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
Cu Cu1 0.7500 0.7500 0.37747(6) 0.02393(18) Uani d S 1 4
N N1 0.2500 0.7500 0.8017(5) 0.0267(5) Uani d S 1 4
N N2 0.5346(3) 0.7500 0.5810(3) 0.0270(4) Uani d S 1 2
N N3 0.7500 0.8958(2) 0.1402(3) 0.0299(4) Uani d S 1 2
C C1 0.3987(3) 0.7500 0.6779(4) 0.0226(4) Uani d S 1 2
C C2 0.7500 1.0397(2) -0.2413(4) 0.0318(5) Uani d S 1 2
H H2A 0.7500 0.9863 -0.3861 0.048 Uiso d SR 1 2
H H2B 0.8562 1.0937 -0.2407 0.048 Uiso d R 1 1
C C3 0.7500 0.95947(19) -0.0270(4) 0.0267(4) Uani d S 1 2
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 0.0242(3) 0.0252(2) 0.0224(3) 0.000 0.000 0.000
N1 0.0233(12) 0.0342(13) 0.0224(12) 0.000 0.000 0.000
N2 0.0241(9) 0.0312(9) 0.0256(8) 0.000 -0.0021(7) 0.000
N3 0.0348(11) 0.0268(10) 0.0281(11) 0.000 0.000 0.0007(7)
C1 0.0258(10) 0.0214(8) 0.0205(9) 0.000 -0.0044(8) 0.000
C2 0.0463(13) 0.0246(10) 0.0245(11) 0.000 0.000 0.0028(9)
C3 0.0307(10) 0.0235(10) 0.0261(11) 0.000 0.000 -0.0014(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Cu1 N2 2_665 . 110.34(11) yes
N2 Cu1 N3 2_665 2_665 111.79(4) ?
N2 Cu1 N3 . 2_665 111.79(4) ?
N2 Cu1 N3 2_665 . 111.79(4) ?
N2 Cu1 N3 . . 111.79(4) yes
N3 Cu1 N3 2_665 . 98.91(11) yes
C1 N1 C1 2_565 . 117.0(3) yes
C1 N2 Cu1 . . 172.85(18) yes
C3 N3 Cu1 . . 166.44(18) ?
N2 C1 N1 . . 176.2(2) yes
C3 C2 H2A . . 109.5 ?
C3 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.6 ?
N3 C3 C2 . . 179.6(2) ?
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 N2 2_665 1.974(2) ?
Cu1 N2 . 1.974(2) yes
Cu1 N3 2_665 2.021(2) ?
Cu1 N3 . 2.021(2) yes
N1 C1 2_565 1.312(3) ?
N1 C1 . 1.312(3) yes
N2 C1 . 1.155(3) yes
N3 C3 . 1.143(3) ?
C3 C2 . 1.457(3) ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
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
N2 Cu1 N3 C3 2_665 117.87(5)
N2 Cu1 N3 C3 . -117.87(5)
N3 Cu1 N3 C3 2_665 0.000(4)
