#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/79/2017967.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_2017967
loop_
_publ_author_name
'Kelley, Annette'
'Akkina, Subhash'
'Devarapally, Goutham K.'
'Nalla, Soujanya'
'Pasam, Divya'
'Madhabushi, Shravani'
'Bond, Marcus R.'
_publ_section_title
;
 Nine compounds containing high-nuclearity
 [CuₙX₂ₙ+2]^2{-^} (n = 4, 5 or 7;
 X = Cl or Br) quasi-planar oligomers
;
_journal_coeditor_code           SK3391
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m22
_journal_page_last               m34
_journal_paper_doi               10.1107/S0108270110049024
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C6 H7 Cl N)2 [Cu7 Br16]'
_chemical_formula_moiety         '2(C6 H7 Cl N +), Br16 Cu7 2-'
_chemical_formula_sum            'C12 H14 Br16 Cl2 Cu7 N2'
_chemical_formula_weight         1980.49
_chemical_name_systematic
;
bis(2-chloro-1-methylpyridinium)
dodeca-μ₂bromido-tetrabromidoheptacuprate(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.9850(10)
_cell_angle_beta                 105.0060(10)
_cell_angle_gamma                100.3740(10)
_cell_formula_units_Z            1
_cell_length_a                   7.23530(10)
_cell_length_b                   10.7361(2)
_cell_length_c                   12.8913(2)
_cell_measurement_reflns_used    5354
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     949.27(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and ORTEPIII (Burnett & Johnson,
1996)
;
_computing_publication_material  'Please provide missing information'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9850
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    20.839
_exptl_absorpt_correction_T_max  0.165
_exptl_absorpt_correction_T_min  0.045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    3.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             897
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.007
_refine_ls_extinction_coef       0.0040(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   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0382
_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)+(0.0468P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                3851
_reflns_number_total             5540
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk3391.cif
_cod_data_source_block           IX
_cod_database_code               2017967
_cod_database_fobs_code          2017967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.5000 1.0000 0.5000 0.0371(2) Uani d S 1 . .
Cu Cu2 0.66624(9) 0.96630(5) 0.26954(4) 0.02747(13) Uani d . 1 . .
Cu Cu3 0.73456(8) 0.91556(5) 0.01312(4) 0.02845(13) Uani d . 1 . .
Cu Cu4 0.83166(8) 0.85687(5) -0.24044(4) 0.02804(13) Uani d . 1 . .
Br Br1 0.61429(7) 1.14129(4) 0.37406(3) 0.02909(11) Uani d . 1 . .
Br Br2 0.54850(7) 0.82832(4) 0.39401(3) 0.02839(11) Uani d . 1 . .
Br Br3 0.71187(6) 1.09738(4) 0.12049(3) 0.02577(11) Uani d . 1 . .
Br Br4 0.63628(7) 0.78398(4) 0.14624(3) 0.02932(11) Uani d . 1 . .
Br Br5 0.81791(6) 1.04245(4) -0.12692(3) 0.02662(11) Uani d . 1 . .
Br Br6 0.76130(7) 0.73570(4) -0.09056(3) 0.03057(12) Uani d . 1 . .
Br Br7 0.93406(6) 0.99782(5) -0.36506(3) 0.03169(12) Uani d . 1 . .
Br Br8 0.80711(9) 0.66457(5) -0.33885(4) 0.04306(15) Uani d . 1 . .
N N1 0.9815(4) 0.5884(3) 0.2396(3) 0.0337(9) Uani d PD 0.834(4) A 1
C C11 1.1112(12) 0.6159(10) 0.1685(7) 0.048(2) Uani d PD 0.834(4) A 1
H H11A 1.2220 0.6798 0.2037 0.072 Uiso calc PR 0.834(4) A 1
H H11B 1.0419 0.6460 0.1028 0.072 Uiso calc PR 0.834(4) A 1
H H11C 1.1543 0.5400 0.1527 0.072 Uiso calc PR 0.834(4) A 1
C C2 0.8181(6) 0.5042(3) 0.21216(19) 0.0349(10) Uani d PD 0.834(4) A 1
Cl Cl1 0.7451(4) 0.4307(2) 0.08112(17) 0.0578(7) Uani d PD 0.834(4) A 1
C C3 0.6988(7) 0.4758(5) 0.2775(4) 0.0433(12) Uani d . 1 A 1
H H3 0.5858 0.4142 0.2560 0.052 Uiso calc R 1 A 1
C C4 0.7500(9) 0.5412(6) 0.3768(4) 0.0519(14) Uani d . 1 A 1
H H4 0.6703 0.5252 0.4231 0.062 Uiso calc R 1 A 1
C C5 0.9188(9) 0.6296(5) 0.4069(4) 0.0501(14) Uani d . 1 A 1
H H5 0.9549 0.6744 0.4737 0.060 Uiso calc R 1 A 1
C C6 1.0335(8) 0.6514(5) 0.3379(4) 0.0431(12) Uani d . 1 A 1
H H6 1.1495 0.7105 0.3586 0.052 Uiso calc R 1 A 1
N N1A 0.8181(6) 0.5042(3) 0.21216(19) 0.0349(10) Uani d P 0.166(4) A 2
C C11A 0.786(5) 0.429(3) 0.1106(15) 0.018(7) Uiso d PD 0.166(4) A 2
C C2A 0.9815(4) 0.5884(3) 0.2396(3) 0.0337(9) Uani d P 0.166(4) A 2
Cl Cl1A 1.1548(15) 0.6178(14) 0.1647(9) 0.039(3) Uiso d PD 0.166(4) A 2
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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
Br1 Cu1 Br2 . . 86.919(13) yes
Br1 Cu1 Br7 . 2_675 88.407(13) yes
Br2 Cu1 Br7 . 2_675 96.163(14) yes
Br1 Cu2 Br2 . . 86.850(19) yes
Br1 Cu2 Br3 . . 93.44(2) yes
Br1 Cu2 Br4 . . 166.59(3) yes
Br1 Cu2 Br5 . 2_675 83.61(2) yes
Br1 Cu2 Br7 . 2_775 95.03(2) yes
Br2 Cu2 Br3 . . 167.62(3) yes
Br2 Cu2 Br4 . . 90.69(2) yes
Br2 Cu2 Br5 . 2_675 88.44(2) yes
Br2 Cu2 Br7 . 2_775 99.73(2) yes
Br3 Cu2 Br4 . . 86.168(19) yes
Br3 Cu2 Br5 . 2_675 79.299(19) yes
Br3 Cu2 Br7 . 2_775 92.58(2) yes
Br4 Cu2 Br5 . 2_675 83.15(2) yes
Br4 Cu2 Br7 . 2_775 98.38(2) yes
Br5 Cu2 Br7 2_675 2_775 171.65(2) yes
Br3 Cu3 Br3 . 2_675 88.89(2) yes
Br3 Cu3 Br4 . . 87.581(19) yes
Br3 Cu3 Br4 2_675 . 91.64(2) yes
Br3 Cu3 Br5 . . 93.67(2) yes
Br3 Cu3 Br5 . 2_775 89.28(2) yes
Br3 Cu3 Br5 2_675 . 85.760(19) yes
Br3 Cu3 Br5 2_675 2_775 172.82(2) yes
Br3 Cu3 Br6 . . 179.09(3) yes
Br3 Cu3 Br6 2_675 . 91.97(2) yes
Br4 Cu3 Br5 . . 177.09(3) yes
Br4 Cu3 Br5 . 2_775 95.22(2) yes
Br4 Cu3 Br6 . . 92.08(2) yes
Br5 Cu3 Br5 . 2_775 87.43(2) yes
Br5 Cu3 Br6 . . 86.71(2) yes
Br5 Cu3 Br6 2_775 . 89.91(2) yes
Br1 Cu4 Br3 2_675 2_775 170.38(2) yes
Br1 Cu4 Br5 2_675 . 88.334(19) yes
Br1 Cu4 Br6 2_675 . 98.05(2) yes
Br1 Cu4 Br7 2_675 . 87.657(19) yes
Br1 Cu4 Br8 2_675 . 87.61(2) yes
Br3 Cu4 Br5 2_775 . 86.689(19) yes
Br3 Cu4 Br6 2_775 . 89.59(2) yes
Br3 Cu4 Br7 2_775 . 84.080(19) yes
Br3 Cu4 Br8 2_775 . 98.34(2) yes
Br5 Cu4 Br6 . . 83.839(19) yes
Br5 Cu4 Br7 . . 89.55(2) yes
Br5 Cu4 Br8 . . 171.60(3) yes
Br6 Cu4 Br7 . . 171.11(3) yes
Br6 Cu4 Br8 . . 89.45(2) yes
Br7 Cu4 Br8 . . 97.63(2) yes
Cu1 Br1 Cu2 . . 92.459(18) yes
Cu1 Br1 Cu4 . 2_675 90.69(2) yes
Cu2 Br1 Cu4 . 2_675 97.54(2) yes
Cu1 Br2 Cu2 . . 93.763(18) yes
Cu2 Br3 Cu3 . . 92.02(2) yes
Cu2 Br3 Cu3 . 2_675 100.58(2) yes
Cu2 Br3 Cu4 . 2_775 85.88(2) yes
Cu3 Br3 Cu3 . 2_675 91.11(2) yes
Cu3 Br3 Cu4 . 2_775 91.69(2) yes
Cu2 Br4 Cu3 . . 92.84(2) yes
Cu2 Br5 Cu3 2_675 . 94.34(2) yes
Cu2 Br5 Cu4 2_675 . 90.47(2) yes
Cu3 Br5 Cu4 . . 94.08(2) yes
Cu3 Br6 Cu4 . . 95.26(2) yes
Cu1 Br7 Cu4 2_675 . 93.24(2) yes
Cu2 Br7 Cu4 2_775 . 97.36(2) yes
C2 N1 C6 . . 118.6(3) ?
C2 N1 C11 . . 122.7(5) ?
C6 N1 C11 . . 118.7(5) ?
N1 C11 H11A . . 109.5 ?
N1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
N1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
N1 C2 C3 . . 123.5(3) ?
N1 C2 Cl1 . . 117.9(3) ?
C3 C2 Cl1 . . 118.5(3) ?
C2 C3 C4 . . 118.0(5) ?
C2 C3 H3 . . 121.0 ?
C4 C3 H3 . . 121.0 ?
C3 C4 C5 . . 119.6(5) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
C4 C5 C6 . . 119.2(5) ?
C4 C5 H5 . . 120.4 ?
C6 C5 H5 . . 120.4 ?
C5 C6 N1 . . 121.1(5) ?
C5 C6 H6 . . 119.4 ?
N1 C6 H6 . . 119.4 ?
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 Br1 . 2.4390(4) yes
Cu1 Br2 . 2.4046(4) yes
Cu1 Br7 2_675 3.1762(4) yes
Cu2 Br1 . 2.4323(6) yes
Cu2 Br2 . 2.4145(6) yes
Cu2 Br3 . 2.4568(6) yes
Cu2 Br4 . 2.4427(6) yes
Cu2 Br5 2_675 3.4929(7) yes
Cu2 Br7 2_775 2.7869(7) yes
Cu3 Br3 . 2.4277(6) yes
Cu3 Br3 2_675 3.2200(7) yes
Cu3 Br4 . 2.4083(6) yes
Cu3 Br5 . 2.4147(6) yes
Cu3 Br5 2_775 3.1355(7) yes
Cu3 Br6 . 2.3942(6) yes
Cu4 Br1 2_675 3.2441(7) yes
Cu4 Br3 2_775 3.2070(7) yes
Cu4 Br5 . 2.4835(6) yes
Cu4 Br6 . 2.4581(6) yes
Cu4 Br7 . 2.3908(6) yes
Cu4 Br8 . 2.3589(7) yes
N1 C11 . 1.47001(11) ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
N1 C6 . 1.356(6) ?
N1 C2 . 1.314(5) ?
C2 Cl1 . 1.760 ?
C2 C3 . 1.356(6) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.377(7) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.367(8) ?
C5 H5 . 0.9300 ?
C5 C6 . 1.361(7) ?
C6 H6 . 0.9300 ?
