#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/80/2018094.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_2018094
loop_
_publ_author_name
'Nalla, Sowjanya'
'Bond, Marcus R.'
_publ_section_title
;
 [CuCl₃(H₂O)]^{-^} complexes aggregated to form hydrate columns in
 methyl-substituted pyridinium or piperidinium salts
;
_journal_coeditor_code           BM3105
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m185
_journal_page_last               m194
_journal_paper_doi               10.1107/S0108270111017306
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C7 H10 N1) [Cu Cl3 (H2 O)]'
_chemical_formula_moiety         'C7 H10 N1 +, H2 Cl3 Cu1 O1 -'
_chemical_formula_sum            'C7 H12 Cl3 Cu N O'
_chemical_formula_weight         296.07
_chemical_name_systematic
;
3,4-dimethylpyridinium aquatrichloridocuprate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.967(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3144(4)
_cell_length_b                   8.8708(2)
_cell_length_c                   8.7761(2)
_cell_measurement_reflns_used    1723
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      2.91
_cell_volume                     1156.99(5)
_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)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0129
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3244
_diffrn_reflns_theta_full        29.6
_diffrn_reflns_theta_max         29.6
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.7
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.572
_refine_ls_extinction_coef       0.0072(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   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1724
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0327
_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)+(0.0450P)²+1.2996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                1485
_reflns_number_total             1724
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bm3105.cif
_cod_data_source_block           II295K
_cod_database_code               2018094
_cod_database_fobs_code          2018094
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.62501(2) 0.0000 0.07768(4) 0.03999(16) Uani d 1 2 . .
Cl Cl1 0.51275(6) 0.0000 0.20481(11) 0.0517(2) Uani d 1 2 . .
Cl Cl2 0.65076(4) 0.25070(6) 0.11599(8) 0.05229(19) Uani d 1 1 . .
O O1 0.71364(19) 0.0000 -0.0534(4) 0.0653(8) Uani d 1 2 . .
H H1W 0.7439(12) 0.0757(6) -0.049(4) 0.078 Uiso d 1 1 . .
C C3 0.8656(3) 0.0000 0.3902(5) 0.0706(13) Uani d 0.50 2 . -1
C C31 0.7961(4) 0.0000 0.4863(8) 0.126(3) Uani d 0.50 2 . -1
H H31A 0.7809 -0.1020 0.5057 0.190 Uiso calc 0.13 1 . -1
H H31B 0.7431 0.0520 0.4298 0.190 Uiso calc 0.13 1 . -1
H H31C 0.8200 0.0501 0.5845 0.190 Uiso calc 0.13 1 . -1
H H31D 0.7818 0.1020 0.5076 0.190 Uiso calc 0.13 1 . -1
H H31E 0.8196 -0.0520 0.5835 0.190 Uiso calc 0.13 1 . -1
H H31F 0.7427 -0.0501 0.4289 0.190 Uiso calc 0.13 1 . -1
C C4 0.8991(2) 0.1290(4) 0.3472(3) 0.0686(8) Uani d 0.50 1 . -1
C C41 0.8674(4) 0.2581(6) 0.4090(7) 0.0603(13) Uani d 0.50 1 . -1
H H41A 0.8932 0.3463 0.3739 0.090 Uiso calc 0.25 1 . -1
H H41B 0.8843 0.2539 0.5216 0.090 Uiso calc 0.25 1 . -1
H H41C 0.8030 0.2626 0.3738 0.090 Uiso calc 0.25 1 . -1
H H41D 0.8271 0.2289 0.4723 0.090 Uiso calc 0.25 1 . -1
H H41E 0.8361 0.3213 0.3246 0.090 Uiso calc 0.25 1 . -1
H H41F 0.9173 0.3125 0.4724 0.090 Uiso calc 0.25 1 . -1
C C5 0.96291(18) 0.1310(3) 0.2574(3) 0.0630(6) Uani d 0.50 1 . -1
H H5 0.9837 0.2221 0.2273 0.076 Uiso calc 0.50 1 . -1
C C6 0.9940(3) 0.0000 0.2150(4) 0.0608(9) Uani d 0.50 2 . -1
H H6 1.0326 0.0000 0.1478 0.073 Uiso d 0.50 2 . -1
C C3A 0.8656(3) 0.0000 0.3902(5) 0.0706(13) Uani d 0.50 2 . -2
C C31A 0.7961(4) 0.0000 0.4863(8) 0.126(3) Uani d 0.50 2 . -2
H H31G 0.7812 -0.1020 0.5064 0.190 Uiso calc 0.13 1 . -2
H H31H 0.7430 0.0513 0.4295 0.190 Uiso calc 0.13 1 . -2
H H31I 0.8199 0.0507 0.5842 0.190 Uiso calc 0.13 1 . -2
H H31J 0.7815 0.1020 0.5070 0.190 Uiso calc 0.13 1 . -2
H H31K 0.8197 -0.0513 0.5838 0.190 Uiso calc 0.13 1 . -2
H H31L 0.7428 -0.0507 0.4292 0.190 Uiso calc 0.13 1 . -2
C C2A 0.8991(2) 0.1290(4) 0.3472(3) 0.0686(8) Uani d 0.50 1 . -2
H H2A 0.8790 0.2202 0.3785 0.082 Uiso calc 0.50 1 . -2
N N1A 0.96291(18) 0.1310(3) 0.2574(3) 0.0630(6) Uani d 0.50 1 . -2
H H1A 0.9821 0.2152 0.2296 0.076 Uiso calc 0.50 1 . -2
C C6A 0.9940(3) 0.0000 0.2150(4) 0.0608(9) Uani d 0.50 2 . -2
H H6A 1.0326 0.0000 0.1478 0.073 Uiso d 0.50 2 . -2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
Cl Cl 0.148 0.159 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.32 1.265 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 '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
Cl1 Cu1 Cl1 . 2_655 86.43(3) yes
Cl1 Cu1 Cl2 . . 93.006(17) yes
Cl1 Cu1 Cl2 2_655 . 101.25(2) yes
Cl2 Cu1 Cl2 . 6 157.01(4) yes
Cl1 Cu1 O1 . . 174.23(11) yes
Cl1 Cu1 O1 2_655 . 87.80(11) yes
Cl2 Cu1 O1 . . 88.12(3) yes
Cu1 Cl1 Cu1 . 2_655 93.57(3) yes
Cu1 O1 H1W . . 116.1(19) ?
H1W O1 H1W 6 . 112(2) ?
C4 C3 C31 . . 121.7(2) ?
C3 C31 H31A . . 109.5 ?
C3 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C3 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C3 C31 H31D . . 109.5 ?
C3 C31 H31E . . 109.5 ?
H31D C31 H31E . . 109.5 ?
C3 C31 H31F . . 109.5 ?
H31D C31 H31F . . 109.5 ?
H31E C31 H31F . . 109.5 ?
C3 C4 C5 . . 122.4(3) ?
C3 C4 C41 . . 113.3(4) ?
C5 C4 C41 . . 124.2(4) ?
C4 C41 H41A . . 109.5 ?
C4 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
C4 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
C4 C41 H41D . . 109.5 ?
C4 C41 H41E . . 109.5 ?
H41D C41 H41E . . 109.5 ?
C4 C41 H41F . . 109.5 ?
H41D C41 H41F . . 109.5 ?
H41E C41 H41F . . 109.5 ?
C6 C5 C4 . . 119.3(3) ?
C6 C5 H5 . . 120.3 ?
C4 C5 H5 . . 120.3 ?
C5 C6 H6 . . 119.9 ?
C5 C6 N1A . 6 119.9(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 Cl1 . 2.2642(8) yes
Cu1 Cl1 2_655 2.8412(11) yes
Cu1 Cl2 . 2.2694(5) yes
Cu1 O1 . 1.980(2) yes
O1 H1W . 0.812(9) ?
C3 C4 . 1.345(4) ?
C3 C31 . 1.509(7) ?
C31 H31A . 0.96 ?
C31 H31B . 0.96 ?
C31 H31C . 0.96 ?
C31 H31D . 0.96 ?
C31 H31E . 0.96 ?
C31 H31F . 0.96 ?
C4 C5 . 1.396(4) ?
C4 C41 . 1.403(6) ?
C41 H41A . 0.96 ?
C41 H41B . 0.96 ?
C41 H41C . 0.96 ?
C41 H41D . 0.96 ?
C41 H41E . 0.96 ?
C41 H41F . 0.96 ?
C5 C6 . 1.342(3) ?
C5 H5 . 0.93 ?
C6 H6 . 0.93 ?
