#------------------------------------------------------------------------------
#$Date: 2017-08-31 16:48:17 +0300 (Thu, 31 Aug 2017) $
#$Revision: 200036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/08/2020869.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_2020869
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      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                 95.8400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4831(3)
_cell_length_b                   7.7267(2)
_cell_length_c                   16.6432(3)
_cell_measurement_reflns_used    3125
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.999
_cell_measurement_theta_min      2.91
_cell_volume                     1852.82(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26631
_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        31.02
_diffrn_reflns_theta_max         31.02
_diffrn_reflns_theta_min         4.64
_exptl_absorpt_coefficient_mu    1.75
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.405
_refine_ls_extinction_coef       0.0246(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0346
_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)+(0.0429P)²+1.1046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.085
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                2250
_reflns_number_total             2939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            og5072sup1_26lutclrt.cif
_cod_data_source_block           26lutclrt
_cod_database_code               2020869
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 0.78550(4) 0.7500 0.04263(13) Uani d S 1 2 . .
Cl Cl1 0.64137(4) 0.67281(8) 0.79331(3) 0.06004(17) Uani d . 1 1 . .
Cl Cl2 0.53700(4) 0.87649(8) 0.63014(3) 0.06239(18) Uani d . 1 1 . .
N N1 0.70831(10) 0.5432(2) 0.62804(9) 0.0418(3) Uani d . 1 1 . .
H H1 0.6896 0.5633 0.6746 0.050 Uiso calc R 1 1 . .
C C2 0.79312(13) 0.5994(2) 0.61480(11) 0.0445(4) Uani d . 1 1 . .
C C21 0.84952(17) 0.6870(3) 0.68284(16) 0.0633(6) Uani d . 1 1 . .
H H21A 0.8150 0.6910 0.7291 0.095 Uiso calc PR 0.50 1 . .
H H21B 0.8639 0.8027 0.6671 0.095 Uiso calc PR 0.50 1 . .
H H21C 0.9061 0.6238 0.6962 0.095 Uiso calc PR 0.50 1 . .
H H21D 0.9083 0.7206 0.6659 0.095 Uiso calc PR 0.50 1 . .
H H21E 0.8594 0.6089 0.7278 0.095 Uiso calc PR 0.50 1 . .
H H21F 0.8172 0.7878 0.6987 0.095 Uiso calc PR 0.50 1 . .
C C3 0.82219(14) 0.5718(3) 0.53938(13) 0.0512(5) Uani d . 1 1 . .
H H3 0.8807 0.6083 0.5283 0.061 Uiso calc R 1 1 . .
C C4 0.76432(16) 0.4902(3) 0.48086(12) 0.0546(5) Uani d . 1 1 . .
H H4 0.7831 0.4746 0.4295 0.066 Uiso calc R 1 1 . .
C C5 0.67803(15) 0.4310(3) 0.49782(12) 0.0511(5) Uani d . 1 1 . .
H H5 0.6393 0.3741 0.4583 0.061 Uiso calc R 1 1 . .
C C6 0.65021(13) 0.4571(2) 0.57318(11) 0.0435(4) Uani d . 1 1 . .
C C61 0.56038(16) 0.3936(3) 0.59925(15) 0.0630(6) Uani d . 1 1 . .
H H61A 0.5560 0.4269 0.6543 0.094 Uiso calc PR 0.50 1 . .
H H61B 0.5578 0.2698 0.5949 0.094 Uiso calc PR 0.50 1 . .
H H61C 0.5097 0.4434 0.5653 0.094 Uiso calc PR 0.50 1 . .
H H61D 0.5263 0.3331 0.5554 0.094 Uiso calc PR 0.50 1 . .
H H61E 0.5245 0.4903 0.6148 0.094 Uiso calc PR 0.50 1 . .
H H61F 0.5726 0.3166 0.6444 0.094 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'
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 . 2_656 134.96(4)
Cl1 Cu1 Cl2 . . 96.52(2)
Cl1 Cu1 Cl2 . 2_656 97.34(2)
Cl2 Cu1 Cl2 . 2_656 143.27(4)
C6 N1 C2 . . 124.43(16)
C6 N1 H1 . . 117.8
C2 N1 H1 . . 117.8
N1 C2 C3 . . 117.93(18)
N1 C2 C21 . . 117.54(18)
C3 C2 C21 . . 124.53(19)
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 . . 119.71(19)
C2 C3 H3 . . 120.1
C4 C3 H3 . . 120.1
C3 C4 C5 . . 120.35(18)
C3 C4 H4 . . 119.8
C5 C4 H4 . . 119.8
C4 C5 C6 . . 119.53(19)
C4 C5 H5 . . 120.2
C6 C5 H5 . . 120.2
C5 C6 N1 . . 118.00(18)
C5 C6 C61 . . 124.25(19)
N1 C6 C61 . . 117.73(18)
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 Cl1 . 2.2736(5)
Cu1 Cl2 . 2.2312(6)
N1 C6 . 1.352(2)
N1 C2 . 1.342(2)
N1 H1 . 0.8600
C2 C3 . 1.381(3)
C2 C21 . 1.490(3)
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 . 1.372(3)
C3 H3 . 0.9300
C4 C5 . 1.387(3)
C4 H4 . 0.9300
C5 C6 . 1.371(3)
C5 H5 . 0.9300
C6 C61 . 1.495(3)
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 2020869
