#------------------------------------------------------------------------------
#$Date: 2017-08-31 16:47:41 +0300 (Thu, 31 Aug 2017) $
#$Revision: 200033 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/08/2020866.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_2020866
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_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 97.5400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5510(3)
_cell_length_b                   7.8249(2)
_cell_length_c                   17.0624(3)
_cell_measurement_reflns_used    3568
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      2.91
_cell_volume                     1925.93(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      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0438
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40655
_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        32.07
_diffrn_reflns_theta_max         32.07
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    9.428
_exptl_absorpt_correction_T_max  0.159
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.804
_refine_diff_density_min         -1.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     96
_refine_ls_number_reflns         3356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0398
_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)+(0.0447P)²+6.0790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                2453
_reflns_number_total             3356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            og5072sup1_26lutbr100k.cif
_cod_data_source_block           26lutbr100k
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2020866
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 0.5 0.81548(8) 0.75 0.01725(14) Uani d S 1 2 . .
Br Br1 0.64826(3) 0.69894(5) 0.802284(19) 0.02023(10) Uani d . 1 1 . .
Br Br2 0.54469(3) 0.91164(5) 0.62839(2) 0.02324(11) Uani d . 1 1 . .
N N1 0.7063(2) 0.5633(4) 0.63017(17) 0.0178(6) Uani d . 1 1 . .
H H1 0.6889 0.5904 0.6748 0.021 Uiso calc R 1 1 . .
C C2 0.7902(2) 0.6155(4) 0.6161(2) 0.0169(7) Uani d . 1 1 . .
C C21 0.8476(3) 0.7115(5) 0.6798(2) 0.0264(8) Uani d . 1 1 . .
H H21A 0.814 0.724 0.7242 0.04 Uiso calc PR 0.5 1 . .
H H21B 0.8619 0.8224 0.6605 0.04 Uiso calc PR 0.5 1 . .
H H21C 0.9041 0.6502 0.6957 0.04 Uiso calc PR 0.5 1 . .
H H21D 0.906 0.7404 0.6627 0.04 Uiso calc PR 0.5 1 . .
H H21E 0.8582 0.642 0.7265 0.04 Uiso calc PR 0.5 1 . .
H H21F 0.8159 0.8142 0.6913 0.04 Uiso calc PR 0.5 1 . .
C C3 0.8178(3) 0.5756(5) 0.5439(2) 0.0204(7) Uani d . 1 1 . .
H H3 0.8759 0.609 0.5324 0.025 Uiso calc R 1 1 . .
C C4 0.7584(3) 0.4855(5) 0.4886(2) 0.0220(7) Uani d . 1 1 . .
H H4 0.7758 0.4618 0.4393 0.026 Uiso calc R 1 1 . .
C C5 0.6727(3) 0.4304(5) 0.5067(2) 0.0218(8) Uani d . 1 1 . .
H H5 0.6335 0.367 0.4703 0.026 Uiso calc R 1 1 . .
C C6 0.6466(3) 0.4707(5) 0.5791(2) 0.0193(7) Uani d . 1 1 . .
C C61 0.5571(3) 0.4142(5) 0.6057(2) 0.0248(8) Uani d . 1 1 . .
H H61A 0.5535 0.4571 0.6579 0.037 Uiso calc PR 0.5 1 . .
H H61B 0.5546 0.2916 0.6062 0.037 Uiso calc PR 0.5 1 . .
H H61C 0.5061 0.4577 0.5699 0.037 Uiso calc PR 0.5 1 . .
H H61D 0.5226 0.3472 0.5648 0.037 Uiso calc PR 0.5 1 . .
H H61E 0.5215 0.5126 0.6165 0.037 Uiso calc PR 0.5 1 . .
H H61F 0.5701 0.3466 0.6528 0.037 Uiso calc PR 0.5 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'
Cu Cu 0.3201 1.2651 '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'
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_656 135.40(3)
Br1 Cu1 Br2 . . 96.261(12)
Br1 Cu1 Br2 . 2_656 97.538(13)
Br2 Cu1 Br2 . 2_656 143.09(4)
C6 N1 C2 . . 124.8(3)
C6 N1 H1 . . 117.6
C2 N1 H1 . . 117.6
N1 C2 C3 . . 118.0(3)
N1 C2 C21 . . 117.6(3)
C3 C2 C21 . . 124.4(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 . . 119.6(3)
C2 C3 H3 . . 120.2
C4 C3 H3 . . 120.2
C3 C4 C5 . . 120.3(3)
C3 C4 H4 . . 119.9
C5 C4 H4 . . 119.9
C4 C5 C6 . . 119.3(3)
C4 C5 H5 . . 120.4
C6 C5 H5 . . 120.4
C5 C6 N1 . . 118.0(3)
C5 C6 C61 . . 123.8(3)
N1 C6 C61 . . 118.1(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 . 2.4034(4)
Cu1 Br2 . 2.3768(4)
N1 C6 . 1.356(5)
N1 C2 . 1.339(5)
N1 H1 . 0.86
C2 C3 . 1.382(5)
C2 C21 . 1.484(5)
C21 H21A . 0.96
C21 H21B . 0.96
C21 H21C . 0.96
C21 H21D . 0.96
C21 H21E . 0.96
C21 H21F . 0.96
C3 C4 . 1.385(5)
C3 H3 . 0.93
C4 C5 . 1.392(5)
C4 H4 . 0.93
C5 C6 . 1.376(5)
C5 H5 . 0.93
C6 C61 . 1.500(5)
C61 H61A . 0.96
C61 H61B . 0.96
C61 H61C . 0.96
C61 H61D . 0.96
C61 H61E . 0.96
C61 H61F . 0.96

_cod_database_fobs_code 2020866
