#------------------------------------------------------------------------------
#$Date: 2017-08-31 16:47:54 +0300 (Thu, 31 Aug 2017) $
#$Revision: 200034 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/08/2020867.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_2020867
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), Br4 Cu'
_chemical_formula_sum            'C14 H20 Br4 Cu N2'
_chemical_formula_weight         599.5
_chemical_name_systematic
;
bis(2,6-dimethylpyridinium) tetrabromidocuprate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.3450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6041(3)
_cell_length_b                   7.9883(2)
_cell_length_c                   17.1986(3)
_cell_measurement_reflns_used    2720
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      2.91
_cell_volume                     1989.96(7)
_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)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26583
_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        28.72
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         4.76
_exptl_absorpt_coefficient_mu    9.125
_exptl_absorpt_correction_T_max  0.176
_exptl_absorpt_correction_T_min  0.115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .21
_exptl_crystal_size_min          .125
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.785
_refine_ls_extinction_coef       0.0047(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0299P)²+3.2871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                2034
_reflns_number_total             2558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            og5072sup1_26lutbrrt.cif
_cod_data_source_block           26lutbrrt
_cod_database_code               2020867
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.5000 0.80484(7) 0.7500 0.04252(14) Uani d S 1 2 . .
Br Br1 0.64681(2) 0.68803(5) 0.801568(17) 0.05525(13) Uani d . 1 1 . .
Br Br2 0.54416(2) 0.90076(5) 0.629655(19) 0.06362(14) Uani d . 1 1 . .
N N1 0.70734(16) 0.5567(3) 0.63033(13) 0.0424(5) Uani d . 1 1 . .
H H1 0.6901 0.5817 0.6749 0.036(7) Uiso calc R 1 1 . .
C C2 0.7903(2) 0.6114(4) 0.61582(18) 0.0450(6) Uani d . 1 1 . .
C C21 0.8472(3) 0.7059(5) 0.6789(2) 0.0665(10) Uani d . 1 1 . .
H H21A 0.8142 0.7154 0.7235 0.100 Uiso calc PR 0.50 1 . .
H H21B 0.8598 0.8157 0.6602 0.100 Uiso calc PR 0.50 1 . .
H H21C 0.9043 0.6478 0.6938 0.100 Uiso calc PR 0.50 1 . .
H H21D 0.9047 0.7372 0.6615 0.100 Uiso calc PR 0.50 1 . .
H H21E 0.8590 0.6369 0.7248 0.100 Uiso calc PR 0.50 1 . .
H H21F 0.8146 0.8048 0.6912 0.100 Uiso calc PR 0.50 1 . .
C C3 0.8166(2) 0.5746(4) 0.54375(19) 0.0532(8) Uani d . 1 1 . .
H H3 0.8737 0.6103 0.5316 0.064 Uiso calc R 1 1 . .
C C4 0.7589(2) 0.4856(5) 0.48976(18) 0.0556(8) Uani d . 1 1 . .
H H4 0.7763 0.4636 0.4406 0.067 Uiso calc R 1 1 . .
C C5 0.6752(2) 0.4286(4) 0.50786(18) 0.0539(8) Uani d . 1 1 . .
H H5 0.6368 0.3659 0.4716 0.065 Uiso calc R 1 1 . .
C C6 0.6487(2) 0.4650(4) 0.57986(17) 0.0450(6) Uani d . 1 1 . .
C C61 0.5607(2) 0.4083(5) 0.6070(2) 0.0656(9) Uani d . 1 1 . .
H H61A 0.5574 0.4497 0.6590 0.098 Uiso calc PR 0.50 1 . .
H H61B 0.5587 0.2882 0.6073 0.098 Uiso calc PR 0.50 1 . .
H H61C 0.5093 0.4506 0.5721 0.098 Uiso calc PR 0.50 1 . .
H H61D 0.5262 0.3426 0.5666 0.098 Uiso calc PR 0.50 1 . .
H H61E 0.5249 0.5041 0.6183 0.098 Uiso calc PR 0.50 1 . .
H H61F 0.5743 0.3418 0.6535 0.098 Uiso calc PR 0.50 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'
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
Br1 Cu1 Br1 . 2_656 134.28(3)
Br1 Cu1 Br2 . . 96.790(11)
Br1 Cu1 Br2 . 2_656 97.627(12)
Br2 Cu1 Br2 . 2_656 142.32(3)
C6 N1 C2 . . 124.7(3)
C6 N1 H1 . . 117.7
C2 N1 H1 . . 117.7
N1 C2 C3 . . 117.5(3)
N1 C2 C21 . . 117.6(3)
C3 C2 C21 . . 124.9(3)
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 C21 H21D . . 109.5
C2 C21 H21E . . 109.5
H21D C21 H21E . . 109.5
C2 C21 H21F . . 109.5
H21D C21 H21F . . 109.5
H21E C21 H21F . . 109.5
C2 C3 C4 . . 120.2(3)
C2 C3 H3 . . 119.9
C4 C3 H3 . . 119.9
C3 C4 C5 . . 120.4(3)
C3 C4 H4 . . 119.8
C5 C4 H4 . . 119.8
C4 C5 C6 . . 119.6(3)
C4 C5 H5 . . 120.2
C6 C5 H5 . . 120.2
C5 C6 N1 . . 117.7(3)
C5 C6 C61 . . 124.7(3)
N1 C6 C61 . . 117.6(3)
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
C6 C61 H61D . . 109.5
C6 C61 H61E . . 109.5
H61D C61 H61E . . 109.5
C6 C61 H61F . . 109.5
H61D C61 H61F . . 109.5
H61E C61 H61F . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 Br1 . 2.4016(4)
Cu1 Br2 . 2.3724(3)
N1 C6 . 1.354(4)
N1 C2 . 1.342(4)
N1 H1 . 0.8600
C2 C3 . 1.375(4)
C2 C21 . 1.486(5)
C21 H21A . 0.9600
C21 H21B . 0.9600
C21 H21C . 0.9600
C21 H21D . 0.9600
C21 H21E . 0.9600
C21 H21F . 0.9600
C3 C4 . 1.371(5)
C3 H3 . 0.9300
C4 C5 . 1.377(5)
C4 H4 . 0.9300
C5 C6 . 1.375(4)
C5 H5 . 0.9300
C6 C61 . 1.493(5)
C61 H61A . 0.9600
C61 H61B . 0.9600
C61 H61C . 0.9600
C61 H61D . 0.9600
C61 H61E . 0.9600
C61 H61F . 0.9600

_cod_database_fobs_code 2020867
