#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/96/2019691.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_2019691
loop_
_publ_author_name
'Karanović, Ljiljana'
'Poleti, Dejan'
'Dordević, Tamara'
_publ_section_title
;
 Ionothermal synthesis and crystal structure of a new organic--inorganic
 hybrid compound: catena-poly[bis(1-ethyl-3-methylimidazolium)
 [hepta-μ-bromido-pentacuprate(I)]]
;
_journal_coeditor_code           BG3188
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1021
_journal_page_last               1024
_journal_paper_doi               10.1107/S205322961402172X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C6 H11 N2)2 [Cu5 Br7]'
_chemical_formula_moiety         '2(C6 H11 N2 +), Br7 Cu5 2-'
_chemical_formula_sum            'C12 H22 Br7 Cu5 N4'
_chemical_formula_weight         1099.41
_chemical_name_common
'1-ethyl-3-methylimidazolium heptabromidopentacupprate(I)'
_chemical_name_systematic
;
catena-Poly[bis(1-ethyl-3-methylimidazolium)
[μ₅-bromido-tri-μ₃-bromido-tri-μ₂-bromido-pentacuprate(I)]]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.736(3)
_cell_length_b                   20.481(4)
_cell_length_c                   10.038(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2618.4(10)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 2002)
;
_computing_data_reduction
;
DENZO-SMN (Otwinowski et al., 2003)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2006) and ATOMS (Dowty, 2000)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SIR97 (Altomare et al., 1999)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ο and θ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            45708
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.989
_exptl_absorpt_coefficient_mu    14.686
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Otwinowski et al., 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.480
_refine_diff_density_min         -1.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0229P)²+9.4671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                2307
_reflns_number_total             3085
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg3188sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019691.cif.'
_cod_original_cell_volume        2618.3(9)
_cod_database_code               2019691
_cod_database_fobs_code          2019691
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.386
_shelx_estimated_absorpt_t_max   0.667
_shelxl_version_number           .2013
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_occupancy
Cu Cu1 0.82942(8) 0.2500 0.26679(10) 0.0514(3) Uani d 1
Cu Cu2 0.70539(6) 0.17479(4) 0.45799(8) 0.0664(2) Uani d 1
Cu Cu3 0.50114(6) 0.17821(4) 0.33841(9) 0.0655(2) Uani d 1
Br Br1 0.89348(5) 0.2500 0.01878(7) 0.03839(17) Uani d 1
Br Br2 0.63702(5) 0.2500 0.21315(7) 0.03377(16) Uani d 1
Br Br3 0.70679(6) 0.2500 0.63700(7) 0.04681(19) Uani d 1
Br Br4 0.88677(4) 0.14820(2) 0.36772(5) 0.03742(12) Uani d 1
Br Br5 0.58741(4) 0.08417(2) 0.42970(5) 0.04333(14) Uani d 1
N N1 0.1721(3) 0.4255(2) 0.5215(4) 0.0375(9) Uani d 1
N N2 0.0522(3) 0.39696(19) 0.6606(4) 0.0381(9) Uani d 1
C C1 0.1105(4) 0.3776(2) 0.5599(5) 0.0374(11) Uani d 1
H H1 0.1084 0.3363 0.5217 0.045 Uiso calc 1
C C2 0.1533(5) 0.4781(3) 0.6006(6) 0.0518(14) Uani d 1
H H2 0.1861 0.5186 0.5956 0.062 Uiso calc 1
C C3 0.0782(4) 0.4605(3) 0.6875(6) 0.0529(15) Uani d 1
H H3 0.0491 0.4866 0.7537 0.063 Uiso calc 1
C C4 0.2476(5) 0.4232(3) 0.4112(5) 0.0555(15) Uani d 1
H H4A 0.2827 0.4645 0.4039 0.083 Uiso calc 1
H H4B 0.2112 0.4139 0.3296 0.083 Uiso calc 1
H H4C 0.2983 0.3895 0.4279 0.083 Uiso calc 1
C C5 -0.0265(4) 0.3568(3) 0.7296(6) 0.0482(13) Uani d 1
H H5A 0.0024 0.3415 0.8134 0.058 Uiso calc 1
H H5B -0.0428 0.3189 0.6755 0.058 Uiso calc 1
C C6 -0.1255(4) 0.3946(3) 0.7561(7) 0.0652(17) Uani d 1
H H6A -0.1752 0.3671 0.8008 0.098 Uiso calc 1
H H6B -0.1547 0.4093 0.6732 0.098 Uiso calc 1
H H6C -0.1097 0.4317 0.8112 0.098 Uiso calc 1
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
Br Br -0.2901 2.4595 '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
Br4 Cu1 Br4 . 7_565 118.15(5) yes
Br4 Cu1 Br2 . . 112.52(3) yes
Br4 Cu1 Br2 7_565 . 112.52(3) yes
Br4 Cu1 Br1 . . 107.61(3) yes
Br4 Cu1 Br1 7_565 . 107.61(3) yes
Br2 Cu1 Br1 . . 95.75(4) yes
Br4 Cu1 Br2 . 6_656 71.24(3) ?
Br4 Cu1 Br2 7_565 6_656 71.24(3) ?
Br2 Cu1 Br2 . 6_656 170.55(4) ?
Br1 Cu1 Br2 . 6_656 74.80(3) ?
Cu3 Cu1 Br2 4 6_656 41.39(2) ?
Cu3 Cu1 Br2 6_656 6_656 41.39(2) ?
Cu2 Cu1 Br2 7_565 6_656 120.38(3) ?
Cu2 Cu1 Br2 . 6_656 120.38(3) ?
Br3 Cu2 Br5 . . 126.63(4) yes
Br3 Cu2 Br4 . . 113.80(4) yes
Br5 Cu2 Br4 . . 111.14(4) yes
Br3 Cu2 Br2 . . 106.70(4) yes
Br5 Cu2 Br2 . . 96.72(3) yes
Br4 Cu2 Br2 . . 94.65(3) yes
Br3 Cu2 Br4 . 7_565 67.39(3) ?
Br5 Cu2 Br4 . 7_565 160.23(4) ?
Br4 Cu2 Br4 . 7_565 67.99(3) ?
Br2 Cu2 Br4 . 7_565 64.16(2) ?
Br5 Cu2 Br5 . 7_565 123.30(3) ?
Br4 Cu2 Br5 . 7_565 116.72(3) ?
Br2 Cu2 Br5 . 7_565 52.118(17) ?
Br1 Cu2 Br5 6_556 7_565 52.230(11) ?
Br4 Cu2 Br5 7_565 7_565 49.708(16) ?
Cu3 Cu2 Br5 6_656 7_565 100.380(19) ?
Br3 Cu2 Br4 . 6_556 123.18(3) ?
Br5 Cu2 Br4 . 6_556 50.37(2) ?
Br4 Cu2 Br4 . 6_556 117.35(3) ?
Br4 Cu2 Br4 7_565 6_556 111.37(2) ?
Br5 Cu2 Br4 7_565 6_556 80.783(16) ?
Br5 Cu3 Br2 . . 109.53(4) yes
Br5 Cu3 Br4 . 6_556 111.73(4) yes
Br2 Cu3 Br4 . 6_556 96.99(4) yes
Br5 Cu3 Br3 . . 74.08(3) ?
Br2 Cu3 Br3 . . 74.59(3) ?
Br4 Cu3 Br3 6_556 . 171.24(3) ?
Br5 Cu3 Br4 . 4_455 171.10(3) ?
Br2 Cu3 Br4 . 4_455 62.06(2) ?
Br4 Cu3 Br4 6_556 4_455 68.21(2) ?
Cu2 Cu3 Br4 7_565 4_455 75.86(2) ?
Br3 Cu3 Br4 . 4_455 104.99(2) ?
Br5 Cu3 Br2 . 6_556 135.71(3) ?
Br2 Cu3 Br2 . 6_556 114.24(3) ?
Br4 Cu3 Br2 6_556 6_556 57.09(2) ?
Br3 Cu3 Br2 . 6_556 123.76(2) ?
Br4 Cu3 Br2 4_455 6_556 52.309(11) ?
C1 N1 C2 . . 108.4(4) ?
C1 N1 C4 . . 126.0(4) ?
C2 N1 C4 . . 125.6(5) ?
C1 N2 C3 . . 107.5(4) ?
C1 N2 C5 . . 125.3(4) ?
C3 N2 C5 . . 127.1(4) ?
N1 C1 N2 . . 109.7(4) ?
N1 C1 H1 . . 125.1 ?
N2 C1 H1 . . 125.1 ?
C3 C2 N1 . . 106.9(5) ?
C3 C2 H2 . . 126.5 ?
N1 C2 H2 . . 126.5 ?
C2 C3 N2 . . 107.4(5) ?
C2 C3 H3 . . 126.3 ?
N2 C3 H3 . . 126.3 ?
N1 C4 H4A . . 109.5 ?
N1 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
N1 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N2 C5 C6 . . 111.5(4) ?
N2 C5 H5A . . 109.3 ?
C6 C5 H5A . . 109.3 ?
N2 C5 H5B . . 109.3 ?
C6 C5 H5B . . 109.3 ?
H5A C5 H5B . . 108.0 ?
C5 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C5 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 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 Br4 . 2.4304(8) yes
Cu1 Br4 7_565 2.4304(8) yes
Cu1 Br2 . 2.5089(13) yes
Cu1 Br1 . 2.6197(13) yes
Cu1 Cu3 4 2.8390(12) yes
Cu1 Cu3 6_656 2.8390(12) yes
Cu1 Cu2 7_565 2.9243(13) yes
Cu1 Cu2 . 2.9243(13) yes
Cu2 Br3 . 2.3667(10) yes
Cu2 Br5 . 2.4049(10) yes
Cu2 Br4 . 2.5405(10) yes
Cu2 Br2 . 3.0283(12) yes
Cu2 Cu3 . 2.8659(12) yes
Cu2 Cu2 7_565 3.0805(17) yes
Cu3 Br5 . 2.3992(9) yes
Cu3 Br1 6_556 2.4692(10) yes
Cu3 Br2 . 2.5958(10) yes
Cu3 Br4 6_556 2.6039(10) yes
Cu3 Cu1 6_556 2.8390(12) yes
Cu3 Cu3 7_565 2.9407(17) yes
Br1 Cu3 4 2.4692(10) ?
Br1 Cu3 6_656 2.4692(10) ?
Br2 Cu3 7_565 2.5958(10) ?
Br2 Cu2 7_565 3.0283(12) ?
Br3 Cu2 7_565 2.3667(10) ?
Br4 Cu3 6_656 2.6039(10) ?
N1 C1 . 1.314(6) yes
N1 C2 . 1.359(6) yes
N1 C4 . 1.468(6) yes
N2 C1 . 1.314(6) yes
N2 C3 . 1.369(6) yes
N2 C5 . 1.470(6) yes
C1 Br4 7_465 3.482(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.344(8) yes
C2 Br4 3_656 3.534(5) ?
C2 H2 . 0.9300 ?
C3 Br4 3_656 3.910(5) ?
C3 Br5 4_456 3.952(6) ?
C3 H3 . 0.9300 ?
C4 Br4 4_455 3.622(5) ?
C4 Cu3 7_565 3.908(6) ?
C4 Br5 4_455 3.987(6) ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
C5 C6 . 1.504(8) yes
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 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
_geom_hbond_publ_flag
C1 H1 Br2 6_556 0.93 2.97 3.803(5) 150.05 yes
C2 H2 Br4 3_656 0.93 2.84 3.534(5) 132.83 yes
C4 H4B Br5 4_455 0.96 3.04 3.987(6) 167.82 yes
C5 H5A Br1 1_456 0.97 3.11 3.774(5) 126.87 yes
C6 H6A Br3 1_455 0.96 3.27 3.842(6) 119.90 yes
