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#$Date: 2016-03-22 11:29:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178901 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/30/4113036.cif $
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#
# 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_4113036
loop_
_publ_author_name
'Xiao-Chun Huang'
'Jie-Peng Zhang'
'Xiao-Ming Chen'
_publ_contact_author
;
       Chen, Xiao-Ming
       School of Chemistry and Chemical Engineering
       Sun Yat-Sen University
       Guangzhou, 510275
       P. R. China
;
_publ_contact_author_email       cescxm@zsu.edu.cn
_publ_contact_author_fax         '86 20 84112245'
_publ_contact_author_phone       86-20-84113986
_publ_section_title
;
 A New Route to Supramolecular Isomers via Molecular Templating: Nanosized
 Molecular Polygons of Copper(I) 2-Methylimidazolates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13218
_journal_page_last               13219
_journal_paper_doi               10.1021/ja045249l
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C39 H48 Cu8 N16'
_chemical_formula_weight         1249.25
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7600(14)
_cell_length_b                   10.8497(7)
_cell_length_c                   21.0042(14)
_cell_measurement_temperature    123(2)
_cell_volume                     4731.0(5)
_computing_cell_refinement
;
         'SAINT-PLUS for Windows NT, Ver. 6.0, Bruker AXS Inc., 1997.'
;
_computing_data_collection
;
         'SMART for Windows NT, Bruker AXS Inc., 1998.'
;
_computing_data_reduction
;
          'SAINT-PLUS for Windows NT, Ver. 6.0,Bruker AXS Inc., 1997.'
;
_computing_molecular_graphics
;
      'XP-Interactive Molecular Graphics, Ver. 6.10, Bruker AXS Inc., 2000.'
;
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15355
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    3.571
_exptl_absorpt_correction_T_max  0.5353
_exptl_absorpt_correction_T_min  0.4139
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0431
_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)+(0.0487P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                4558
_reflns_number_total             5321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja045249lsi20040812_020015_2.cif
_cod_data_source_block           compound_2
_cod_database_code               4113036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, 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
Cu1 Cu 0.36285(3) 0.17740(6) 0.35945(3) 0.02748(16) Uani 1 1 d .
Cu2 Cu 0.18496(3) -0.17329(6) 0.25649(3) 0.02762(16) Uani 1 1 d .
Cu3 Cu 0.18240(3) -0.56871(5) 0.07399(3) 0.02523(15) Uani 1 1 d .
Cu4 Cu 0.36257(3) -0.91458(6) -0.02235(3) 0.02909(16) Uani 1 1 d .
N1 N 0.44619(19) 0.2422(4) 0.3666(2) 0.0282(10) Uani 1 1 d .
N2 N 0.2850(2) 0.0938(4) 0.3470(2) 0.0263(10) Uani 1 1 d .
N3 N 0.2162(2) -0.0416(4) 0.3041(2) 0.0246(10) Uani 1 1 d .
N4 N 0.1561(2) -0.2934(4) 0.1998(2) 0.0269(10) Uani 1 1 d .
N5 N 0.1543(2) -0.4486(4) 0.1301(2) 0.0265(10) Uani 1 1 d .
N6 N 0.2144(2) -0.6967(4) 0.0230(2) 0.0250(10) Uani 1 1 d .
N7 N 0.2839(2) -0.8334(4) -0.0146(2) 0.0256(10) Uani 1 1 d .
N8 N 0.44591(18) -0.9753(4) -0.0216(2) 0.0268(9) Uani 1 1 d .
C1 C 0.5000 0.1804(7) 0.3521(4) 0.0276(16) Uani 1 2 d S
C2 C 0.4674(2) 0.3520(5) 0.3930(3) 0.0313(12) Uani 1 1 d .
H2 H 0.4407 0.4165 0.4086 0.038 Uiso 1 1 calc R
C3 C 0.5000 0.0538(7) 0.3207(4) 0.0362(18) Uani 1 2 d S
H3A H 0.5000 0.0617 0.2752 0.043 Uiso 1 2 d SR
H3B H 0.4626 0.0087 0.3341 0.043 Uiso 1 1 d R
C4 C 0.2786(2) -0.0141(5) 0.3139(3) 0.0247(12) Uani 1 1 d .
C5 C 0.1824(3) 0.0526(5) 0.3322(3) 0.0250(11) Uani 1 1 d .
H5 H 0.1368 0.0589 0.3334 0.030 Uiso 1 1 calc R
C6 C 0.2233(3) 0.1342(5) 0.3576(3) 0.0260(11) Uani 1 1 d .
H6 H 0.2117 0.2077 0.3793 0.031 Uiso 1 1 calc R
C7 C 0.3332(3) -0.0875(5) 0.2898(3) 0.0339(14) Uani 1 1 d .
H7A H 0.3168 -0.1614 0.2684 0.051 Uiso 1 1 calc R
H7B H 0.3608 -0.1119 0.3254 0.051 Uiso 1 1 calc R
H7C H 0.3581 -0.0381 0.2595 0.051 Uiso 1 1 calc R
C8 C 0.1909(2) -0.3703(6) 0.1657(3) 0.0270(10) Uani 1 1 d .
C9 C 0.0918(3) -0.4138(5) 0.1435(3) 0.0357(14) Uani 1 1 d .
H9 H 0.0542 -0.4501 0.1259 0.043 Uiso 1 1 calc R
C10 C 0.0926(3) -0.3207(5) 0.1854(3) 0.0339(13) Uani 1 1 d .
H10 H 0.0558 -0.2803 0.2024 0.041 Uiso 1 1 calc R
C11 C 0.2627(2) -0.3739(7) 0.1651(3) 0.0334(11) Uani 1 1 d .
H11A H 0.2796 -0.3098 0.1934 0.050 Uiso 1 1 calc R
H11B H 0.2783 -0.3596 0.1217 0.050 Uiso 1 1 calc R
H11C H 0.2775 -0.4549 0.1799 0.050 Uiso 1 1 calc R
C12 C 0.2763(2) -0.7292(5) 0.0172(3) 0.0258(12) Uani 1 1 d .
C13 C 0.2232(3) -0.8708(5) -0.0323(3) 0.0257(12) Uani 1 1 d .
H13 H 0.2130 -0.9416 -0.0569 0.031 Uiso 1 1 calc R
C14 C 0.1801(3) -0.7872(5) -0.0079(3) 0.0286(12) Uani 1 1 d .
H14 H 0.1346 -0.7911 -0.0117 0.034 Uiso 1 1 calc R
C15 C 0.3312(3) -0.6555(6) 0.0444(3) 0.0374(14) Uani 1 1 d .
H15A H 0.3141 -0.5843 0.0677 0.056 Uiso 1 1 calc R
H15B H 0.3591 -0.6268 0.0098 0.056 Uiso 1 1 calc R
H15C H 0.3562 -0.7073 0.0736 0.056 Uiso 1 1 calc R
C16 C 0.5000 -0.9126(7) -0.0379(4) 0.0294(18) Uani 1 2 d S
C17 C 0.4674(2) -1.0836(4) 0.0061(3) 0.0285(11) Uani 1 1 d .
H17 H 0.4407 -1.1474 0.0224 0.034 Uiso 1 1 calc R
C18 C 0.5000 -0.7874(8) -0.0680(5) 0.049(2) Uani 1 2 d S
H18A H 0.5000 -0.7959 -0.1135 0.059 Uiso 1 2 d SR
H18B H 0.5375 -0.7422 -0.0549 0.059 Uiso 1 1 d R
C19 C 0.5000 -0.2205(15) 0.1967(8) 0.126(6) Uiso 1 2 d SD
H19 H 0.5000 -0.1536 0.2259 0.151 Uiso 1 2 calc SR
C20 C 0.4449(6) -0.2736(10) 0.1736(5) 0.132(5) Uiso 1 1 d D
H20 H 0.4048 -0.2404 0.1870 0.158 Uiso 1 1 calc R
C21 C 0.4439(5) -0.3722(9) 0.1321(4) 0.101(3) Uiso 1 1 d D
H21 H 0.4039 -0.4023 0.1165 0.121 Uiso 1 1 calc R
C22 C 0.5000 -0.4266(11) 0.1132(6) 0.074(3) Uiso 1 2 d SD
C23 C 0.5000 -0.5270(15) 0.0677(8) 0.126(6) Uiso 1 2 d SD
H23A H 0.5000 -0.4961 0.0248 0.151 Uiso 1 2 d SR
H23B H 0.4626 -0.5772 0.0745 0.151 Uiso 1 1 d R
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'
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
N2 Cu1 N1 172.1(2) . .
N2 Cu1 Cu2 82.51(14) . 8
N1 Cu1 Cu2 99.63(14) . 8
N3 Cu2 N4 172.8(2) . .
N3 Cu2 Cu1 98.52(14) . 8_545
N4 Cu2 Cu1 88.62(14) . 8_545
N5 Cu3 N6 175.2(2) . .
N5 Cu3 Cu4 86.21(14) . 8
N6 Cu3 Cu4 98.54(14) . 8
N8 Cu4 N7 170.7(2) . .
N8 Cu4 Cu3 95.39(15) . 8_545
N7 Cu4 Cu3 85.77(14) . 8_545
C1 N1 C2 104.9(4) . .
C1 N1 Cu1 124.4(4) . .
C2 N1 Cu1 130.4(3) . .
C4 N2 C6 105.3(5) . .
C4 N2 Cu1 124.8(4) . .
C6 N2 Cu1 128.9(4) . .
C4 N3 C5 105.1(4) . .
C4 N3 Cu2 126.1(4) . .
C5 N3 Cu2 128.6(3) . .
C8 N4 C10 105.6(4) . .
C8 N4 Cu2 127.9(4) . .
C10 N4 Cu2 126.5(4) . .
C8 N5 C9 103.9(4) . .
C8 N5 Cu3 127.8(4) . .
C9 N5 Cu3 128.3(4) . .
C12 N6 C14 105.4(5) . .
C12 N6 Cu3 126.0(4) . .
C14 N6 Cu3 128.0(4) . .
C12 N7 C13 106.3(4) . .
C12 N7 Cu4 123.5(4) . .
C13 N7 Cu4 129.8(4) . .
C16 N8 C17 105.4(4) . .
C16 N8 Cu4 126.4(4) . .
C17 N8 Cu4 127.3(3) . .
N1 C1 N1 113.2(7) 4_655 .
N1 C1 C3 123.4(3) 4_655 .
N1 C1 C3 123.4(3) . .
C2 C2 N1 108.5(3) 4_655 .
N3 C4 N2 111.3(5) . .
N3 C4 C7 124.5(5) . .
N2 C4 C7 124.2(5) . .
C6 C5 N3 109.8(5) . .
C5 C6 N2 108.5(5) . .
N4 C8 N5 112.8(4) . .
N4 C8 C11 124.8(6) . .
N5 C8 C11 122.4(5) . .
C10 C9 N5 109.2(5) . .
C9 C10 N4 108.4(5) . .
N7 C12 N6 112.7(5) . .
N7 C12 C15 123.8(5) . .
N6 C12 C15 123.6(5) . .
C14 C13 N7 107.5(5) . .
C13 C14 N6 108.1(5) . .
N8 C16 N8 111.8(6) . 4_655
N8 C16 C18 124.1(3) . .
N8 C16 C18 124.1(3) 4_655 .
C17 C17 N8 108.7(3) 4_655 .
C20 C19 C20 113.3(18) . 4_655
C19 C20 C21 124.3(14) . .
C22 C21 C20 120.3(12) . .
C21 C22 C21 117.2(13) 4_655 .
C21 C22 C23 121.1(7) 4_655 .
C21 C22 C23 121.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.871(5) .
Cu1 N1 1.874(4) .
Cu1 Cu2 2.8786(9) 8
Cu2 N3 1.861(4) .
Cu2 N4 1.865(4) .
Cu2 Cu1 2.8786(9) 8_545
Cu3 N5 1.851(5) .
Cu3 N6 1.875(4) .
Cu3 Cu4 2.7863(9) 8
Cu4 N8 1.851(4) .
Cu4 N7 1.864(4) .
Cu4 Cu3 2.7863(9) 8_545
N1 C1 1.338(6) .
N1 C2 1.387(7) .
N2 C4 1.367(7) .
N2 C6 1.372(7) .
N3 C4 1.344(6) .
N3 C5 1.373(6) .
N4 C8 1.315(7) .
N4 C10 1.384(7) .
N5 C8 1.364(7) .
N5 C9 1.381(7) .
N6 C12 1.338(6) .
N6 C14 1.376(7) .
N7 C12 1.322(7) .
N7 C13 1.374(7) .
N8 C16 1.356(6) .
N8 C17 1.386(6) .
C1 N1 1.338(6) 4_655
C1 C3 1.523(10) .
C2 C2 1.352(10) 4_655
C4 C7 1.476(7) .
C5 C6 1.338(7) .
C8 C11 1.492(6) .
C9 C10 1.339(7) .
C12 C15 1.506(8) .
C13 C14 1.373(8) .
C16 N8 1.356(6) 4_655
C16 C18 1.498(11) .
C17 C17 1.356(10) 4_655
C19 C20 1.369(8) .
C19 C20 1.369(8) 4_655
C20 C21 1.381(8) .
C21 C22 1.365(8) .
C22 C21 1.365(8) 4_655
C22 C23 1.450(19) .
