#------------------------------------------------------------------------------
#$Date: 2017-08-31 16:47:25 +0300 (Thu, 31 Aug 2017) $
#$Revision: 200032 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/08/2020865.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_2020865
loop_
_publ_author_name
'Kelley, Annette'
'Nalla, Sowjanya'
'Bond, Marcus R.'
_publ_section_title
;
 The square-planar to flattened-tetrahedral CuX42−(X= Cl, Br)
 structural phase transition in 1,2,6-trimethylpyridinium salts
;
_journal_coeditor_code           OG5072
_journal_issue                   1
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_page_first              48
_journal_page_last               60
_journal_paper_doi               10.1107/S205252061402664X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         '2(C7 H10 N), Cl4 Cu'
_chemical_formula_sum            'C14 H20 Cl4 Cu N2'
_chemical_formula_weight         421.66
_chemical_name_systematic
;
bis(2,6-dimethylpyridinium) tetrachloridocuprate(II)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9587(3)
_cell_length_b                   7.88580(10)
_cell_length_c                   13.8774(3)
_cell_measurement_reflns_used    3360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.999
_cell_measurement_theta_min      2.91
_cell_volume                     1855.87(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59438
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        31.01
_diffrn_reflns_theta_max         31.01
_diffrn_reflns_theta_min         4.44
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_T_max  0.663
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             860
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .13
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.635
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0372P)²+0.9700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                2386
_reflns_number_total             2952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            og5072sup1_26lut100kortho.cif
_cod_data_source_block           26lut100kortho
_cod_original_cell_volume        1855.86(6)
_cod_database_code               2020865
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, 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 0.19627(4) 0.7500 0.01663(8) Uani d S 1 2 . .
Cl Cl1 0.45461(2) 0.32504(6) 0.61533(3) 0.02629(11) Uani d . 1 1 . .
Cl Cl2 0.61240(2) 0.08444(5) 0.69371(3) 0.02111(10) Uani d . 1 1 . .
N N1 0.61990(8) 0.35374(18) 0.50879(10) 0.0182(3) Uani d . 1 1 . .
H H1 0.5746(13) 0.352(3) 0.5401(15) 0.026(5) Uiso d . 1 1 . .
C C2 0.68341(9) 0.4285(2) 0.54931(12) 0.0195(3) Uani d . 1 1 . .
C C21 0.67203(10) 0.5189(3) 0.64282(13) 0.0271(4) Uani d . 1 1 . .
H H21A 0.6433 0.4474 0.6864 0.060(8) Uiso calc R 1 1 . .
H H21B 0.6430 0.6216 0.6320 0.043(7) Uiso calc R 1 1 . .
H H21C 0.7225 0.5458 0.6701 0.048(7) Uiso calc R 1 1 . .
C C3 0.75438(10) 0.4191(2) 0.50011(13) 0.0230(3) Uani d . 1 1 . .
H H3 0.7997(13) 0.470(3) 0.5290(16) 0.030(5) Uiso d . 1 1 . .
C C4 0.75726(11) 0.3391(2) 0.41113(14) 0.0258(4) Uani d . 1 1 . .
H H4 0.8055(14) 0.332(3) 0.3788(16) 0.030(6) Uiso d . 1 1 . .
C C5 0.69008(11) 0.2682(2) 0.37218(13) 0.0238(3) Uani d . 1 1 . .
H H5 0.6899(13) 0.214(3) 0.3147(16) 0.030(6) Uiso d . 1 1 . .
C C6 0.61975(10) 0.2748(2) 0.42278(12) 0.0206(3) Uani d . 1 1 . .
C C61 0.54389(11) 0.1994(3) 0.38877(15) 0.0317(4) Uani d . 1 1 . .
H H61A 0.5303 0.1046 0.4289 0.088(11) Uiso calc R 1 1 . .
H H61B 0.5497 0.1618 0.3233 0.082(10) Uiso calc R 1 1 . .
H H61C 0.5029 0.2832 0.3922 0.071(10) 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
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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'
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'
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
Cl1 Cu1 Cl1 . 4_656 126.65(3)
Cl1 Cu1 Cl2 . . 100.259(15)
Cl2 Cu1 Cl1 . 4_656 100.094(15)
Cl2 Cu1 Cl2 . 4_656 133.65(3)
C6 N1 C2 . . 124.93(15)
C6 N1 H1 . . 115.4(14)
C2 N1 H1 . . 119.7(14)
N1 C2 C3 . . 117.66(15)
N1 C2 C21 . . 117.85(14)
C3 C2 C21 . . 124.47(15)
C2 C21 H21A . . 109.5
C2 C21 H21B . . 109.5
H21A C21 H21B . . 109.5
C2 C21 H21C . . 109.5
H21A C21 H21C . . 109.5
H21B C21 H21C . . 109.5
C2 C3 C4 . . 119.56(16)
C2 C3 H3 . . 118.0(13)
C4 C3 H3 . . 122.4(13)
C3 C4 C5 . . 120.27(16)
C3 C4 H4 . . 119.1(14)
C5 C4 H4 . . 120.6(14)
C4 C5 C6 . . 119.82(17)
C4 C5 H5 . . 122.7(14)
C6 C5 H5 . . 117.5(14)
C5 C6 N1 . . 117.72(16)
C5 C6 C61 . . 124.51(16)
N1 C6 C61 . . 117.77(15)
C6 C61 H61A . . 109.5
C6 C61 H61B . . 109.5
H61A C61 H61B . . 109.5
C6 C61 H61C . . 109.5
H61A C61 H61C . . 109.5
H61B C61 H61C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 Cl1 . 2.2619(4)
Cu1 Cl2 . 2.2409(4)
N1 C6 . 1.346(2)
N1 C2 . 1.351(2)
N1 H1 . 0.88(2)
C2 C3 . 1.386(2)
C2 C21 . 1.493(2)
C21 H21A . 0.9600
C21 H21B . 0.9600
C21 H21C . 0.9600
C3 C4 . 1.388(3)
C3 H3 . 0.95(2)
C4 C5 . 1.379(3)
C4 H4 . 0.93(2)
C5 C6 . 1.385(2)
C5 H5 . 0.90(2)
C6 C61 . 1.494(2)
C61 H61A . 0.9600
C61 H61B . 0.9600
C61 H61C . 0.9600

_cod_database_fobs_code 2020865
