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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/59/4305974.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4305974
loop_
_publ_author_name
'Firas Awwadi'
'Roger D. Willett'
'Brendan Twamley'
'Ryan Schneider'
'Christopher P. Landee'
_publ_contact_author_address
;University Research Office
103 Morrill Hall
University of Idaho
Moscow, 
ID, 83844-3010
USA
;
_publ_contact_author_email       btwamley@uidaho.edu
_publ_contact_author_fax         '208 885 5752'
_publ_contact_author_name        'Brendan Twamley'
_publ_contact_author_phone       '208 885 2847'
_publ_section_title
;
Strong Rail Spin1/2 Antiferromagnetic Ladder Systems:
(Dimethylammonium)(3,5-Dimethylpyridinium)CuX4, X = Cl, Br
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9327
_journal_page_last               9332
_journal_paper_doi               10.1021/ic800905e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C14 H25.4 Cl15 Cu7.51 N4 O1.28'
_chemical_formula_weight         1279.20
_chemical_name_common            {[Cu(TIM)]2[Cu13Cl30(H2O)4]xH2O}n
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.7616(10)
_cell_angle_beta                 107.115(2)
_cell_angle_gamma                109.192(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4539(13)
_cell_length_b                   9.7873(13)
_cell_length_c                   10.9255(15)
_cell_measurement_reflns_used    9369
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.27
_cell_volume                     877.0(2)
_computing_cell_refinement       'Bruker SAINT+ v. 6.45a'
_computing_data_collection       'Bruker SMART v. 5.630'
_computing_data_reduction        'Bruker SAINT+ v. 6.45a'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_diffrn_ambient_temperature      89(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SAMRT APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12823
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.629
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2001'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3178
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0228
_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)+(0.0305P)²+0.8611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                2974
_reflns_number_total             3178
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic800905e_si_002_1.cif
_cod_data_source_block           bt850
_cod_original_formula_sum        'C14 H25.40 Cl15 Cu7.51 N4 O1.28'
_cod_database_code               4305974
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.940(2) 0.4476(19) 1.0416(17) 0.045(6) Uiso 0.145(8) 1 d P . .
Cu1 Cu 0.5000 0.5000 1.0000 0.0109(3) Uani 0.508(2) 2 d SP . .
Cu2 Cu 0.83653(3) 0.49145(3) 1.21824(3) 0.01478(9) Uani 1 1 d . . .
Cu3 Cu 1.17632(3) 0.49077(3) 1.42287(3) 0.01431(9) Uani 1 1 d . . .
Cu4 Cu 1.50008(4) 0.52975(3) 1.68257(3) 0.01625(9) Uani 1 1 d D . .
Cu5 Cu 0.5000 0.0000 1.0000 0.01440(11) Uani 1 2 d S . .
Cl1 Cl 0.77515(7) 0.63854(7) 1.09109(6) 0.01715(14) Uani 1 1 d . . .
Cl2 Cl 0.58006(7) 0.31420(7) 1.12755(6) 0.01584(14) Uani 1 1 d . . .
Cl3 Cl 1.10532(8) 0.64364(8) 1.30165(7) 0.02302(16) Uani 1 1 d . . .
Cl4 Cl 0.90834(7) 0.34567(7) 1.34854(6) 0.01475(14) Uani 1 1 d . . .
Cl5 Cl 1.43736(7) 0.65967(7) 1.52943(6) 0.01522(14) Uani 1 1 d . . .
Cl6 Cl 1.23279(7) 0.36213(7) 1.57859(6) 0.01385(13) Uani 1 1 d . . .
Cl7 Cl 1.76396(7) 0.67114(7) 1.75281(6) 0.01755(14) Uani 1 1 d . . .
C2 C 0.2506(3) 0.0047(3) 0.7920(3) 0.0163(5) Uani 1 1 d U . .
C2' C 0.0986(3) 0.0061(3) 0.7024(3) 0.0214(6) Uani 1 1 d U . .
H2'A H 0.0215 -0.0067 0.7476 0.032 Uiso 1 1 calc R . .
H2'B H 0.0528 -0.0763 0.6206 0.032 Uiso 1 1 calc R . .
H2'C H 0.1214 0.1024 0.6801 0.032 Uiso 1 1 calc R . .
C3 C 0.3871(3) 0.0194(3) 0.7422(3) 0.0165(5) Uani 1 1 d U . .
C3' C 0.3607(4) 0.0213(3) 0.6015(3) 0.0248(6) Uani 1 1 d U . .
H3'A H 0.4602 0.0336 0.5852 0.037 Uiso 1 1 calc R . .
H3'B H 0.3303 0.1052 0.5848 0.037 Uiso 1 1 calc R . .
H3'C H 0.2742 -0.0737 0.5417 0.037 Uiso 1 1 calc R . .
C5 C 0.6619(3) 0.0422(3) 0.7998(3) 0.0228(6) Uani 1 1 d U . .
H5A H 0.6696 0.1024 0.7351 0.027 Uiso 1 1 calc R . .
H5B H 0.6544 -0.0586 0.7586 0.027 Uiso 1 1 calc R . .
C6 C 0.8131(3) 0.1183(3) 0.9255(3) 0.0229(6) Uani 1 1 d U . .
H6A H 0.9082 0.1466 0.8992 0.028 Uiso 1 1 calc R . .
H6B H 0.8115 0.2123 0.9724 0.028 Uiso 1 1 calc R . .
C7 C 0.8336(3) 0.0238(3) 1.0221(3) 0.0194(6) Uani 1 1 d U . .
H7A H 0.8183 -0.0770 0.9731 0.023 Uiso 1 1 calc R . .
H7B H 0.9445 0.0718 1.0897 0.023 Uiso 1 1 calc R . .
N1 N 0.2822(2) -0.0073(2) 0.9112(2) 0.0140(4) Uani 1 1 d . . .
N4 N 0.5161(3) 0.0263(2) 0.8285(2) 0.0166(5) Uani 1 1 d . . .
Cl8 Cl 1.5388(4) 0.3789(2) 1.8163(3) 0.0166(4) Uani 0.50 1 d P . 1
O8 O 1.5318(12) 0.4128(9) 1.8151(9) 0.0166(4) Uani 0.50 1 d PD . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Cu1 O8 180.000(2) 2_768 1_454 ?
O8 Cu1 Cl1 92.4(3) 2_768 . ?
O8 Cu1 Cl1 87.6(3) 1_454 . ?
O8 Cu1 Cl1 87.6(3) 2_768 2_667 ?
O8 Cu1 Cl1 92.4(3) 1_454 2_667 ?
Cl1 Cu1 Cl1 180.0 . 2_667 ?
O8 Cu1 Cl8 8.29(18) 2_768 2_768 ?
O8 Cu1 Cl8 171.71(18) 1_454 2_768 ?
Cl1 Cu1 Cl8 92.35(8) . 2_768 ?
Cl1 Cu1 Cl8 87.65(8) 2_667 2_768 ?
O8 Cu1 Cl8 171.71(18) 2_768 1_454 ?
O8 Cu1 Cl8 8.29(18) 1_454 1_454 ?
Cl1 Cu1 Cl8 87.65(8) . 1_454 ?
Cl1 Cu1 Cl8 92.35(8) 2_667 1_454 ?
Cl8 Cu1 Cl8 180.000(1) 2_768 1_454 ?
O8 Cu1 Cl2 96.89(16) 2_768 2_667 ?
O8 Cu1 Cl2 83.11(16) 1_454 2_667 ?
Cl1 Cu1 Cl2 97.65(2) . 2_667 ?
Cl1 Cu1 Cl2 82.35(2) 2_667 2_667 ?
Cl8 Cu1 Cl2 88.68(4) 2_768 2_667 ?
Cl8 Cu1 Cl2 91.32(4) 1_454 2_667 ?
O8 Cu1 Cl2 83.11(16) 2_768 . ?
O8 Cu1 Cl2 96.89(16) 1_454 . ?
Cl1 Cu1 Cl2 82.35(2) . . ?
Cl1 Cu1 Cl2 97.65(2) 2_667 . ?
Cl8 Cu1 Cl2 91.32(4) 2_768 . ?
Cl8 Cu1 Cl2 88.68(4) 1_454 . ?
Cl2 Cu1 Cl2 180.0 2_667 . ?
Cl1 Cu2 Cl2 92.34(3) . . ?
Cl1 Cu2 Cl4 177.97(3) . . ?
Cl2 Cu2 Cl4 89.52(2) . . ?
Cl1 Cu2 Cl3 92.29(3) . . ?
Cl2 Cu2 Cl3 172.13(3) . . ?
Cl4 Cu2 Cl3 85.77(2) . . ?
Cl4 Cu3 Cl3 86.29(2) . . ?
Cl4 Cu3 Cl5 169.29(3) . . ?
Cl3 Cu3 Cl5 93.46(3) . . ?
Cl4 Cu3 Cl6 91.50(2) . . ?
Cl3 Cu3 Cl6 167.71(3) . . ?
Cl5 Cu3 Cl6 86.47(2) . . ?
Cl4 Cu3 Cl7 95.65(2) . 2_868 ?
Cl3 Cu3 Cl7 98.48(3) . 2_868 ?
Cl5 Cu3 Cl7 94.97(2) . 2_868 ?
Cl6 Cu3 Cl7 93.76(3) . 2_868 ?
O8 Cu4 Cl7 92.9(3) . . ?
O8 Cu4 Cl8 6.3(3) . . ?
Cl7 Cu4 Cl8 92.88(8) . . ?
O8 Cu4 Cl5 174.2(3) . . ?
Cl7 Cu4 Cl5 92.33(3) . . ?
Cl8 Cu4 Cl5 173.63(8) . . ?
O8 Cu4 Cl6 89.7(3) . . ?
Cl7 Cu4 Cl6 170.09(3) . . ?
Cl8 Cu4 Cl6 88.63(8) . . ?
Cl5 Cu4 Cl6 85.62(2) . . ?
N4 Cu5 N4 180.000(1) 2_657 . ?
N4 Cu5 N1 98.71(9) 2_657 . ?
N4 Cu5 N1 81.29(9) . . ?
N4 Cu5 N1 81.29(9) 2_657 2_657 ?
N4 Cu5 N1 98.71(9) . 2_657 ?
N1 Cu5 N1 180.000(1) . 2_657 ?
Cu2 Cl1 Cu1 96.77(2) . . ?
Cu2 Cl2 Cu1 87.79(2) . . ?
Cu3 Cl3 Cu2 93.76(3) . . ?
Cu3 Cl4 Cu2 94.05(2) . . ?
Cu3 Cl5 Cu4 94.40(2) . . ?
Cu3 Cl6 Cu4 93.47(2) . . ?
Cu4 Cl7 Cu3 96.46(3) . 2_868 ?
N1 C2 C2' 126.9(2) . . ?
N1 C2 C3 114.0(2) . . ?
C2' C2 C3 119.0(2) . . ?
C2 C2' H2'A 109.5 . . ?
C2 C2' H2'B 109.5 . . ?
H2'A C2' H2'B 109.5 . . ?
C2 C2' H2'C 109.5 . . ?
H2'A C2' H2'C 109.5 . . ?
H2'B C2' H2'C 109.5 . . ?
N4 C3 C3' 126.2(2) . . ?
N4 C3 C2 114.6(2) . . ?
C3' C3 C2 119.2(2) . . ?
C3 C3' H3'A 109.5 . . ?
C3 C3' H3'B 109.5 . . ?
H3'A C3' H3'B 109.5 . . ?
C3 C3' H3'C 109.5 . . ?
H3'A C3' H3'C 109.5 . . ?
H3'B C3' H3'C 109.5 . . ?
N4 C5 C6 111.6(2) . . ?
N4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C7 C6 C5 115.0(2) . . ?
C7 C6 H6A 108.5 . . ?
C5 C6 H6A 108.5 . . ?
C7 C6 H6B 108.5 . . ?
C5 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
N1 C7 C6 111.4(2) 2_657 . ?
N1 C7 H7A 109.3 2_657 . ?
C6 C7 H7A 109.3 . . ?
N1 C7 H7B 109.3 2_657 . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C2 N1 C7 122.8(2) . 2_657 ?
C2 N1 Cu5 115.04(17) . . ?
C7 N1 Cu5 122.14(16) 2_657 . ?
C3 N4 C5 122.8(2) . . ?
C3 N4 Cu5 114.85(17) . . ?
C5 N4 Cu5 122.26(17) . . ?
Cu4 Cl8 Cu1 99.22(7) . 1_656 ?
Cu4 O8 Cu1 113.7(3) . 1_656 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2 O2 1.82(3) 2_767 ?
Cu1 O8 2.214(9) 2_768 ?
Cu1 O8 2.214(9) 1_454 ?
Cu1 Cl1 2.3112(7) . ?
Cu1 Cl1 2.3112(7) 2_667 ?
Cu1 Cl8 2.358(3) 2_768 ?
Cu1 Cl8 2.358(3) 1_454 ?
Cu1 Cl2 2.6226(7) 2_667 ?
Cu1 Cl2 2.6226(7) . ?
Cu2 Cl1 2.2412(7) . ?
Cu2 Cl2 2.2731(7) . ?
Cu2 Cl4 2.2825(7) . ?
Cu2 Cl3 2.2894(7) . ?
Cu3 Cl4 2.2730(7) . ?
Cu3 Cl3 2.2768(7) . ?
Cu3 Cl5 2.2845(7) . ?
Cu3 Cl6 2.3075(7) . ?
Cu3 Cl7 2.6103(7) 2_868 ?
Cu4 O8 1.992(6) . ?
Cu4 Cl7 2.2377(7) . ?
Cu4 Cl8 2.2683(18) . ?
Cu4 Cl5 2.3082(7) . ?
Cu4 Cl6 2.3204(7) . ?
Cu5 N4 1.972(2) 2_657 ?
Cu5 N4 1.972(2) . ?
Cu5 N1 1.973(2) . ?
Cu5 N1 1.973(2) 2_657 ?
Cl7 Cu3 2.6103(7) 2_868 ?
C2 N1 1.281(3) . ?
C2 C2' 1.488(4) . ?
C2 C3 1.515(4) . ?
C2' H2'A 0.9800 . ?
C2' H2'B 0.9800 . ?
C2' H2'C 0.9800 . ?
C3 N4 1.276(3) . ?
C3 C3' 1.488(4) . ?
C3' H3'A 0.9800 . ?
C3' H3'B 0.9800 . ?
C3' H3'C 0.9800 . ?
C5 N4 1.467(3) . ?
C5 C6 1.522(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.517(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N1 1.464(3) 2_657 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N1 C7 1.464(3) 2_657 ?
Cl8 Cu1 2.358(3) 1_656 ?
O8 Cu1 2.214(9) 1_656 ?
