#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/81/4108180.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_4108180
loop_
_publ_author_name
'Wen Zhang'
'Ren-Gen Xiong'
'Songping D. Huang'
_publ_section_title
;
 3D Framework Containing Cu4Br4 Cubane as Connecting Node with Strong
 Ferroelectricity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10468
_journal_page_last               10469
_journal_paper_doi               10.1021/ja803021v
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C33 H60 Br8 Cu8 N6, 1.5(H2 O), 1.5(H2 O)'
_chemical_formula_sum            'C33 H66 Br8 Cu8 N6 O3'
_chemical_formula_weight         1742.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           143
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   15.2582(18)
_cell_length_b                   15.2582(18)
_cell_length_c                   6.6579(9)
_cell_measurement_reflns_used    1558
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      21.81
_cell_measurement_theta_min      2.66
_cell_volume                     1342.4(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7411
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    9.094
_exptl_absorpt_correction_T_max  0.284
_exptl_absorpt_correction_T_min  0.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.04P)²+1.33P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                2827
_reflns_number_total             3487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803021v-file001.cif
_cod_data_source_block           270427d
_cod_original_sg_symbol_Hall     'P 3   '
_cod_original_sg_symbol_H-M      'P 3 '
_cod_database_code               4108180
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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
Br1 Br 0.0000 1.0000 0.7784(2) 0.0484(5) Uani 1 3 d S
Br2 Br 0.17179(10) 1.10906(8) 0.28696(15) 0.0490(3) Uani 1 1 d .
Br3 Br 0.3333 0.6667 0.5102(2) 0.0412(4) Uani 1 3 d S
Br4 Br 0.46107(8) 0.62527(8) 0.01127(15) 0.0484(3) Uani 1 1 d .
C1 C 0.1502(7) 0.8646(7) 0.8211(13) 0.036(2) Uani 1 1 d .
H1A H 0.1119 0.8866 0.9021 0.043 Uiso 1 1 calc R
H1B H 0.2031 0.8662 0.9044 0.043 Uiso 1 1 calc R
C2 C 0.0802(7) 0.7565(7) 0.7469(16) 0.042(2) Uani 1 1 d .
H2 H 0.0268 0.7566 0.6650 0.050 Uiso 1 1 calc R
C3 C 0.1780(7) 0.7936(9) 0.4525(17) 0.051(3) Uani 1 1 d .
H3A H 0.1259 0.8004 0.3830 0.061 Uiso 1 1 calc R
H3B H 0.2106 0.7709 0.3573 0.061 Uiso 1 1 calc R
C4 C 0.2539(8) 0.8923(6) 0.5461(18) 0.048(3) Uani 1 1 d .
H4A H 0.2968 0.8822 0.6396 0.057 Uiso 1 1 calc R
H4B H 0.2964 0.9398 0.4435 0.057 Uiso 1 1 calc R
C5 C 0.0281(7) 0.6830(6) 0.9330(14) 0.041(2) Uani 1 1 d .
H5A H -0.0259 0.6193 0.8859 0.062 Uiso 1 1 calc R
H5B H 0.0014 0.7129 1.0233 0.062 Uiso 1 1 calc R
H5C H 0.0774 0.6725 1.0019 0.062 Uiso 1 1 calc R
C6 C 0.2608(10) 1.0351(8) 0.7474(19) 0.059(3) Uani 1 1 d .
H6A H 0.2198 1.0670 0.7595 0.071 Uiso 1 1 calc R
H6B H 0.2765 1.0239 0.8829 0.071 Uiso 1 1 calc R
C7 C 0.3543(9) 1.1071(8) 0.6552(14) 0.056(3) Uani 1 1 d .
H7 H 0.3897 1.0891 0.5665 0.067 Uiso 1 1 calc R
C8 C 0.3848(9) 1.1998(9) 0.7071(18) 0.066(3) Uani 1 1 d .
H8A H 0.3466 1.2140 0.7964 0.079 Uiso 1 1 calc R
H8B H 0.4448 1.2521 0.6551 0.079 Uiso 1 1 calc R
C9 C 0.0668(7) 0.6079(6) 0.5560(13) 0.034(2) Uani 1 1 d .
H9A H 0.1036 0.5905 0.4602 0.041 Uiso 1 1 calc R
H9B H 0.0496 0.5632 0.6709 0.041 Uiso 1 1 calc R
C10 C -0.0302(7) 0.5958(7) 0.4585(13) 0.041(2) Uani 1 1 d .
H10 H -0.0307 0.6534 0.4141 0.050 Uiso 1 1 calc R
C11 C -0.1151(7) 0.5041(6) 0.4349(13) 0.040(2) Uani 1 1 d .
H11A H -0.1160 0.4457 0.4784 0.048 Uiso 1 1 calc R
H11B H -0.1723 0.4997 0.3753 0.048 Uiso 1 1 calc R
Cu1 Cu 0.08418(11) 0.94849(10) 0.4884(2) 0.0504(4) Uani 1 1 d .
Cu2 Cu 0.0000 1.0000 1.1429(3) 0.0414(5) Uani 1 3 d S
Cu3 Cu 0.24242(10) 0.71179(9) 0.78351(19) 0.0422(3) Uani 1 1 d .
Cu4 Cu 0.3333 0.6667 0.1269(3) 0.0373(4) Uani 1 3 d S
N1 N 0.1947(7) 0.9318(6) 0.6535(12) 0.042(2) Uani 1 1 d .
N2 N 0.1335(6) 0.7203(6) 0.6239(11) 0.0356(17) Uani 1 1 d .
O1 O 0.6078(12) 0.2467(11) 0.775(2) 0.080(6) Uani 0.50 1 d P
H1C H 0.6688 0.2808 0.8145 0.120 Uiso 0.50 1 d PR
H1D H 0.5752 0.1959 0.8514 0.120 Uiso 0.50 1 d PR
O2 O 0.4964(10) 0.2231(11) 0.137(2) 0.059(4) Uani 0.50 1 d P
H2A H 0.5114 0.1853 0.0689 0.088 Uiso 0.50 1 d PR
H2B H 0.4326 0.1982 0.1374 0.088 Uiso 0.50 1 d PR
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'
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'
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
Cu2 Br1 Cu1 136.84(4) . 3_465
Cu2 Br1 Cu1 136.84(4) . 2_675
Cu1 Br1 Cu1 72.65(7) 3_465 2_675
Cu2 Br1 Cu1 136.84(4) . .
Cu1 Br1 Cu1 72.65(7) 3_465 .
Cu1 Br1 Cu1 72.65(7) 2_675 .
Cu1 Br2 Cu2 72.42(6) 2_675 1_554
Cu1 Br2 Cu1 78.08(7) 2_675 .
Cu2 Br2 Cu1 71.63(6) 1_554 .
Cu4 Br3 Cu3 134.82(4) . .
Cu4 Br3 Cu3 134.82(4) . 3_565
Cu3 Br3 Cu3 75.80(6) . 3_565
Cu4 Br3 Cu3 134.82(4) . 2_665
Cu3 Br3 Cu3 75.80(6) . 2_665
Cu3 Br3 Cu3 75.80(6) 3_565 2_665
Cu4 Br4 Cu3 72.89(5) . 3_564
Cu4 Br4 Cu3 68.33(5) . 2_664
Cu3 Br4 Cu3 74.61(7) 3_564 2_664
N1 C1 C2 110.2(8) . .
N1 C1 H1A 109.6 . .
C2 C1 H1A 109.6 . .
N1 C1 H1B 109.6 . .
C2 C1 H1B 109.6 . .
H1A C1 H1B 108.1 . .
N2 C2 C1 111.8(8) . .
N2 C2 C5 110.5(7) . .
C1 C2 C5 110.0(8) . .
N2 C2 H2 108.2 . .
C1 C2 H2 108.2 . .
C5 C2 H2 108.2 . .
N2 C3 C4 105.5(9) . .
N2 C3 H3A 110.6 . .
C4 C3 H3A 110.6 . .
N2 C3 H3B 110.6 . .
C4 C3 H3B 110.6 . .
H3A C3 H3B 108.8 . .
N1 C4 C3 106.5(8) . .
N1 C4 H4A 110.4 . .
C3 C4 H4A 110.4 . .
N1 C4 H4B 110.4 . .
C3 C4 H4B 110.4 . .
H4A C4 H4B 108.6 . .
C2 C5 H5A 109.5 . .
C2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 N1 120.7(10) . .
C7 C6 H6A 107.2 . .
N1 C6 H6A 107.2 . .
C7 C6 H6B 107.2 . .
N1 C6 H6B 107.2 . .
H6A C6 H6B 106.8 . .
C8 C7 C6 113.6(11) . .
C8 C7 H7 123.2 . .
C6 C7 H7 123.2 . .
C7 C8 H8A 120.0 . .
C7 C8 H8B 120.0 . .
H8A C8 H8B 120.0 . .
C10 C9 N2 108.3(7) . .
C10 C9 H9A 110.0 . .
N2 C9 H9A 110.0 . .
C10 C9 H9B 110.0 . .
N2 C9 H9B 110.0 . .
H9A C9 H9B 108.4 . .
C11 C10 C9 122.4(8) . .
C11 C10 H10 118.8 . .
C9 C10 H10 118.8 . .
C10 C11 H11A 120.0 . .
C10 C11 H11B 120.0 . .
H11A C11 H11B 120.0 . .
N1 Cu1 Br2 132.1(2) . 3_465
N1 Cu1 Br2 109.0(2) . .
Br2 Cu1 Br2 106.14(8) 3_465 .
N1 Cu1 Br1 100.9(2) . .
Br2 Cu1 Br1 102.84(6) 3_465 .
Br2 Cu1 Br1 101.56(5) . .
N1 Cu1 Cu2 156.5(3) . 1_554
Br2 Cu1 Cu2 54.17(4) 3_465 1_554
Br2 Cu1 Cu2 53.82(4) . 1_554
Br1 Cu1 Cu2 98.64(6) . 1_554
Br1 Cu2 Br2 112.66(6) . 1_556
Br1 Cu2 Br2 112.66(6) . 3_466
Br2 Cu2 Br2 106.10(6) 1_556 3_466
Br1 Cu2 Br2 112.66(6) . 2_676
Br2 Cu2 Br2 106.10(6) 1_556 2_676
Br2 Cu2 Br2 106.10(6) 3_466 2_676
Br1 Cu2 Cu1 141.80(4) . 2_676
Br2 Cu2 Cu1 53.41(5) 1_556 2_676
Br2 Cu2 Cu1 105.54(8) 3_466 2_676
Br2 Cu2 Cu1 54.55(5) 2_676 2_676
Br1 Cu2 Cu1 141.80(4) . 1_556
Br2 Cu2 Cu1 54.55(5) 1_556 1_556
Br2 Cu2 Cu1 53.41(5) 3_466 1_556
Br2 Cu2 Cu1 105.54(8) 2_676 1_556
Cu1 Cu2 Cu1 64.77(6) 2_676 1_556
Br1 Cu2 Cu1 141.80(4) . 3_466
Br2 Cu2 Cu1 105.54(8) 1_556 3_466
Br2 Cu2 Cu1 54.55(5) 3_466 3_466
Br2 Cu2 Cu1 53.41(5) 2_676 3_466
Cu1 Cu2 Cu1 64.77(6) 2_676 3_466
Cu1 Cu2 Cu1 64.77(6) 1_556 3_466
N2 Cu3 Br4 130.7(2) . 2_666
N2 Cu3 Br3 102.4(2) . .
Br4 Cu3 Br3 107.09(6) 2_666 .
N2 Cu3 Br4 112.0(2) . 3_566
Br4 Cu3 Br4 101.10(7) 2_666 3_566
Br3 Cu3 Br4 99.59(5) . 3_566
N2 Cu3 Cu4 157.3(2) . 1_556
Br4 Cu3 Cu4 53.19(4) 2_666 1_556
Br3 Cu3 Cu4 96.13(6) . 1_556
Br4 Cu3 Cu4 51.12(3) 3_566 1_556
Br4 Cu4 Br4 110.64(5) 2_665 3_565
Br4 Cu4 Br4 110.64(5) 2_665 .
Br4 Cu4 Br4 110.64(5) 3_565 .
Br4 Cu4 Br3 108.28(5) 2_665 .
Br4 Cu4 Br3 108.28(5) 3_565 .
Br4 Cu4 Br3 108.28(5) . .
Br4 Cu4 Cu3 53.92(5) 2_665 1_554
Br4 Cu4 Cu3 60.55(5) 3_565 1_554
Br4 Cu4 Cu3 110.26(8) . 1_554
Br3 Cu4 Cu3 141.30(4) . 1_554
Br4 Cu4 Cu3 110.26(8) 2_665 2_664
Br4 Cu4 Cu3 53.92(5) 3_565 2_664
Br4 Cu4 Cu3 60.55(5) . 2_664
Br3 Cu4 Cu3 141.30(4) . 2_664
Cu3 Cu4 Cu3 65.56(6) 1_554 2_664
Br4 Cu4 Cu3 60.55(5) 2_665 3_564
Br4 Cu4 Cu3 110.26(8) 3_565 3_564
Br4 Cu4 Cu3 53.92(5) . 3_564
Br3 Cu4 Cu3 141.30(4) . 3_564
Cu3 Cu4 Cu3 65.56(6) 1_554 3_564
Cu3 Cu4 Cu3 65.56(6) 2_664 3_564
C1 N1 C4 104.4(8) . .
C1 N1 C6 104.6(8) . .
C4 N1 C6 113.1(9) . .
C1 N1 Cu1 111.5(6) . .
C4 N1 Cu1 118.4(6) . .
C6 N1 Cu1 104.1(7) . .
C2 N2 C3 106.1(8) . .
C2 N2 C9 113.7(7) . .
C3 N2 C9 113.7(7) . .
C2 N2 Cu3 111.3(6) . .
C3 N2 Cu3 111.4(5) . .
C9 N2 Cu3 100.7(6) . .
H1C O1 H1D 109.5 . .
H2A O2 H2B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Cu2 2.427(3) .
Br1 Cu1 2.6467(19) 3_465
Br1 Cu1 2.6467(19) 2_675
Br1 Cu1 2.6467(19) .
Br2 Cu1 2.465(2) 2_675
Br2 Cu2 2.4895(15) 1_554
Br2 Cu1 2.5125(17) .
Br3 Cu4 2.552(3) .
Br3 Cu3 2.5818(19) .
Br3 Cu3 2.5818(19) 3_565
Br3 Cu3 2.5818(19) 2_665
Br4 Cu4 2.4538(13) .
Br4 Cu3 2.4771(17) 3_564
Br4 Cu3 2.7446(16) 2_664
C1 N1 1.435(12) .
C1 C2 1.531(12) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N2 1.445(13) .
C2 C5 1.591(13) .
C2 H2 0.9800 .
C3 N2 1.502(13) .
C3 C4 1.502(14) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 N1 1.495(13) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.432(17) .
C6 N1 1.517(14) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.295(14) .
C7 H7 0.9300 .
C8 H8A 0.9300 .
C8 H8B 0.9300 .
C9 C10 1.540(13) .
C9 N2 1.560(11) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.360(13) .
C10 H10 0.9300 .
C11 H11A 0.9300 .
C11 H11B 0.9300 .
Cu1 N1 2.132(8) .
Cu1 Br2 2.465(2) 3_465
Cu1 Cu2 2.927(2) 1_554
Cu2 Br2 2.4895(15) 1_556
Cu2 Br2 2.4895(15) 3_466
Cu2 Br2 2.4895(15) 2_676
Cu2 Cu1 2.927(2) 2_676
Cu2 Cu1 2.927(2) 1_556
Cu2 Cu1 2.927(2) 3_466
Cu3 N2 2.031(9) .
Cu3 Br4 2.4771(17) 2_666
Cu3 Br4 2.7446(16) 3_566
Cu3 Cu4 2.929(2) 1_556
Cu4 Br4 2.4538(13) 2_665
Cu4 Br4 2.4538(13) 3_565
Cu4 Cu3 2.929(2) 1_554
Cu4 Cu3 2.929(2) 2_664
Cu4 Cu3 2.929(2) 3_564
O1 H1C 0.8500 .
O1 H1D 0.8500 .
O2 H2A 0.8499 .
O2 H2B 0.8500 .
