#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:52:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178921 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/50/4115086.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_4115086
loop_
_publ_author_name
'Heba Abourahma'
'Brian Moulton'
'Victor Kravtsov'
'Michael J. Zaworotko'
_publ_section_title
;
 Supramolecular Isomerism in Coordination Compounds: Nanoscale Molecular
 Hexagons and Chains
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9990
_journal_page_last               9991
_journal_paper_doi               10.1021/ja027371v
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C41 H40 Cu N6 O9 S0.08'
_chemical_formula_weight         827.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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            12
_cell_length_a                   35.023(4)
_cell_length_b                   35.023(4)
_cell_length_c                   9.9711(13)
_cell_measurement_reflns_used    7673
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.35
_cell_measurement_theta_min      2.15
_cell_volume                     10592(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1249
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14506
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             5164
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7267
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          1.132
_refine_ls_shift/su_mean         0.211
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1500P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2176
_refine_ls_wR_factor_ref         0.2357
_reflns_number_gt                5117
_reflns_number_total             7267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja027371v_s1_2.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4115086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Cu1 Cu 0.86884(8) 0.13803(9) -0.07982(16) 0.0780(7) Uani 1 1 d D . .
O1WA O 0.8587(3) 0.1395(3) 0.1134(9) 0.060(3) Uani 1 1 d D A .
O1A O 0.8126(4) 0.0823(4) -0.0928(18) 0.105(5) Uani 1 1 d D A .
O2A O 0.7790(6) 0.1234(4) -0.1137(16) 0.096(5) Uani 1 1 d D A .
O3A O 0.6231(5) 0.0477(5) -0.1528(19) 0.103(5) Uani 1 1 d D . .
O4A O 0.5849(4) -0.0225(5) -0.1229(13) 0.102(6) Uani 1 1 d D . .
O5A O 0.7277(4) -0.0776(4) -0.1276(16) 0.091(5) Uani 1 1 d D A .
O6A O 0.6544(4) -0.1106(3) -0.1295(13) 0.076(4) Uani 1 1 d D A .
N1A N 0.6187(4) 0.0120(5) -0.1325(11) 0.074(5) Uani 1 1 d D . .
C1A C 0.7794(4) 0.0878(4) -0.1061(16) 0.061(5) Uani 1 1 d D . .
C2A C 0.7363(4) 0.0447(4) -0.1191(17) 0.063(5) Uani 1 1 d D A .
C3A C 0.7359(4) 0.0055(4) -0.1245(15) 0.056(4) Uani 1 1 d D . .
H3A H 0.7626 0.0047 -0.1298 0.067 Uiso 1 1 calc R A .
C4A C 0.6946(4) -0.0338(3) -0.1221(14) 0.050(4) Uani 1 1 d D A .
C5A C 0.6556(5) -0.0333(5) -0.1244(15) 0.069(6) Uani 1 1 d D . .
H5A H 0.6278 -0.0596 -0.1201 0.083 Uiso 1 1 calc R A .
C6A C 0.6593(4) 0.0078(4) -0.1331(16) 0.059(4) Uani 1 1 d D A .
C7A C 0.6985(5) 0.0459(5) -0.1268(15) 0.074(6) Uani 1 1 d D . .
H7A H 0.6994 0.0735 -0.1278 0.089 Uiso 1 1 calc R A .
C8A C 0.6928(5) -0.0782(4) -0.1242(18) 0.074(6) Uani 1 1 d D . .
O1MA O 0.9056(7) 0.1010(8) -0.073(2) 0.160(9) Uani 1 1 d . A .
C1MA C 0.9566(5) 0.1336(7) -0.029(3) 0.153(11) Uani 1 1 d . . .
H1M1 H 0.9724 0.1171 -0.0292 0.230 Uiso 1 1 calc R A .
H1M2 H 0.9575 0.1451 0.0613 0.230 Uiso 1 1 calc R . .
H1M3 H 0.9705 0.1582 -0.0925 0.230 Uiso 1 1 calc R . .
Cu2 Cu 0.73161(10) -0.13073(8) -0.11523(16) 0.0777(7) Uani 1 1 d D . .
O1WB O 0.7209(4) -0.1417(4) -0.3087(9) 0.071(3) Uani 1 1 d D A .
O1B O 0.7307(4) -0.1863(3) -0.1035(13) 0.074(4) Uani 1 1 d D A .
O2B O 0.6581(4) -0.2220(5) -0.0836(15) 0.093(5) Uani 1 1 d D A .
O3B O 1.0451(5) 0.4252(4) -0.0492(19) 0.124(7) Uani 1 1 d D . .
O4B O 0.9752(4) 0.3921(4) -0.0742(17) 0.105(6) Uani 1 1 d D . .
O5B O 0.9217(4) 0.1938(3) -0.0657(12) 0.069(4) Uani 1 1 d D A .
O6B O 0.8876(4) 0.2313(6) -0.0796(17) 0.098(5) Uani 1 1 d D A .
N1B N 1.0090(5) 0.3912(4) -0.0587(19) 0.102(7) Uani 1 1 d D . .
C1B C 0.6943(5) -0.2200(6) -0.080(2) 0.090(8) Uani 1 1 d D . .
C2B C 1.0451(4) 0.3084(4) -0.0759(12) 0.051(4) Uani 1 1 d D . .
C3B C 1.0051(4) 0.2711(5) -0.0816(16) 0.060(5) Uani 1 1 d D . .
H3B H 1.0041 0.2438 -0.0949 0.072 Uiso 1 1 calc R . .
C4B C 0.9642(4) 0.2709(5) -0.0685(16) 0.075(6) Uani 1 1 d D A .
C5B C 0.9667(4) 0.3112(3) -0.0668(14) 0.056(4) Uani 1 1 d D . .
H5B H 0.9406 0.3132 -0.0623 0.067 Uiso 1 1 calc R . .
C6B C 1.0078(4) 0.3492(3) -0.0718(15) 0.055(4) Uani 1 1 d D . .
C7B C 1.0457(4) 0.3477(4) -0.0670(17) 0.071(5) Uani 1 1 d D . .
H7B H 1.0730 0.3743 -0.0573 0.086 Uiso 1 1 calc R . .
C8B C 0.9214(4) 0.2283(4) -0.0748(18) 0.064(5) Uiso 1 1 d D . .
O2WB O 0.8063(8) -0.0938(8) -0.153(2) 0.156(8) Uiso 1 1 d . A .
O1DB O 0.7435(16) -0.1184(8) 0.058(3) 0.40(4) Uani 1 1 d D A .
S1DB S 0.7410(9) -0.1453(11) 0.155(3) 0.54(3) Uani 1 1 d D A .
C1DB C 0.6811(17) -0.1794(14) 0.217(7) 1.4(4) Uani 1 1 d D . .
H1D1 H 0.6634 -0.2016 0.1490 2.157 Uiso 1 1 calc R A .
H1D2 H 0.6690 -0.1599 0.2314 2.157 Uiso 1 1 calc R . .
H1D3 H 0.6803 -0.1942 0.3010 2.157 Uiso 1 1 calc R . .
C2DB C 0.758(2) -0.1094(16) 0.311(2) 0.77(10) Uani 1 1 d D . .
H2D1 H 0.7901 -0.0915 0.3150 1.159 Uiso 1 1 calc R A .
H2D2 H 0.7469 -0.1282 0.3909 1.159 Uiso 1 1 calc R . .
H2D3 H 0.7452 -0.0900 0.3076 1.159 Uiso 1 1 calc R . .
O1DA O 0.8723(6) 0.1434(5) -0.2752(9) 0.134(6) Uani 1 1 d D A 1
S1DA S 0.8466(4) 0.1181(3) -0.3687(7) 0.299(11) Uani 1 1 d D A 1
C1DA C 0.8653(16) 0.1326(11) -0.5469(17) 0.28(3) Uani 1 1 d D A 1
H1D4 H 0.8639 0.1588 -0.5732 0.418 Uiso 1 1 calc R A 1
H1D5 H 0.8460 0.1079 -0.6055 0.418 Uiso 1 1 calc R A 1
H1D6 H 0.8957 0.1385 -0.5553 0.418 Uiso 1 1 calc R A 1
C2DA C 0.8531(9) 0.0660(8) -0.370(2) 0.142(9) Uani 1 1 d D A 1
H2D4 H 0.8506 0.0551 -0.2777 0.213 Uiso 1 1 calc R A 1
H2D5 H 0.8821 0.0737 -0.4062 0.213 Uiso 1 1 calc R A 1
H2D6 H 0.8300 0.0431 -0.4253 0.213 Uiso 1 1 calc R A 1
O1M O 1.1982(5) -0.0030(5) -0.3511(18) 0.136(6) Uani 1 1 d D . .
C1M C 1.1620(6) -0.0018(5) -0.421(3) 0.131(10) Uani 1 1 d D . .
O2M O 1.1999(13) 0.1868(13) 0.232(5) 0.52(6) Uani 1 1 d D . .
C2M C 1.1680(10) 0.140(2) 0.263(9) 1.19(18) Uani 1 1 d D . .
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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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_3
O5B Cu1 O1DA 89.6(6) .
O5B Cu1 O1A 176.8(6) .
O1DA Cu1 O1A 90.8(7) .
O5B Cu1 O1WA 89.8(5) .
O1DA Cu1 O1WA 168.0(6) .
O1A Cu1 O1WA 89.2(6) .
O5B Cu1 O1MA 92.7(7) .
O1DA Cu1 O1MA 93.5(8) .
O1A Cu1 O1MA 90.4(8) .
O1WA Cu1 O1MA 98.5(7) .
C1A O1A Cu1 113.2(9) .
C8A O5A Cu2 122.5(10) .
O3A N1A O4A 127.6(13) .
O3A N1A C6A 118.0(11) .
O4A N1A C6A 114.0(12) .
O2A C1A O1A 128.3(13) .
O2A C1A C2A 118.8(13) .
O1A C1A C2A 112.9(12) .
C7A C2A C3A 121.0(11) .
C7A C2A C1A 118.5(11) .
C3A C2A C1A 120.5(12) .
C2A C3A C4A 117.8(10) .
C5A C4A C3A 121.9(9) .
C5A C4A C8A 118.6(10) .
C3A C4A C8A 119.4(9) .
C4A C5A C6A 116.0(11) .
C7A C6A C5A 122.9(10) .
C7A C6A N1A 116.5(11) .
C5A C6A N1A 120.2(11) .
C2A C7A C6A 119.9(11) .
O5A C8A O6A 129.0(12) .
O5A C8A C4A 117.2(11) .
O6A C8A C4A 113.7(12) .
C1MA O1MA Cu1 110.5(11) .
O1DB Cu2 O5A 87.1(7) .
O1DB Cu2 O1B 94.0(6) .
O5A Cu2 O1B 175.7(6) .
O1DB Cu2 O1WB 177.4(14) .
O5A Cu2 O1WB 91.5(6) .
O1B Cu2 O1WB 87.5(5) .
O1DB Cu2 O2WB 87.7(17) .
O5A Cu2 O2WB 93.3(8) .
O1B Cu2 O2WB 91.0(8) .
O1WB Cu2 O2WB 90.2(7) .
O1DB Cu2 S1DB 21.9(7) .
O5A Cu2 S1DB 108.0(8) .
O1B Cu2 S1DB 72.7(8) .
O1WB Cu2 S1DB 160.0(8) .
O2WB Cu2 S1DB 93.1(8) .
C1B O1B Cu2 117.2(10) .
C8B O5B Cu1 121.6(9) .
O4B N1B O3B 122.0(15) .
O4B N1B C6B 118.6(13) .
O3B N1B C6B 118.7(13) .
O2B C1B O1B 125.4(14) .
O2B C1B C2B 114.0(15) 2_645
O1B C1B C2B 119.1(11) 2_645
C3B C2B C7B 117.1(12) .
C3B C2B C1B 120.3(11) 3_765
C7B C2B C1B 122.6(11) 3_765
C2B C3B C4B 123.4(12) .
C5B C4B C3B 116.5(11) .
C5B C4B C8B 123.0(9) .
C3B C4B C8B 120.0(11) .
C4B C5B C6B 119.3(11) .
C7B C6B C5B 121.8(10) .
C7B C6B N1B 120.1(11) .
C5B C6B N1B 117.2(10) .
C6B C7B C2B 121.0(11) .
O5B C8B O6B 124.7(13) .
O5B C8B C4B 119.0(11) .
O6B C8B C4B 116.1(12) .
S1DB O1DB Cu2 127.9(19) .
O1DB S1DB C2DB 104(2) .
O1DB S1DB C1DB 110(3) .
C2DB S1DB C1DB 92(2) .
O1DB S1DB Cu2 30.2(13) .
C2DB S1DB Cu2 134.0(14) .
C1DB S1DB Cu2 103(3) .
S1DA O1DA Cu1 131.7(10) .
O1DA S1DA C1DA 118.1(14) .
O1DA S1DA C2DA 106.2(14) .
C1DA S1DA C2DA 93.5(16) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5B 1.909(11) .
Cu1 O1DA 1.955(9) .
Cu1 O1A 1.965(11) .
Cu1 O1WA 1.964(8) .
Cu1 O1MA 2.239(13) .
O1A C1A 1.275(14) .
O2A C1A 1.258(13) .
O3A N1A 1.196(13) .
O4A N1A 1.201(14) .
O5A C8A 1.212(14) .
O5A Cu2 1.936(14) .
O6A C8A 1.254(13) .
N1A C6A 1.501(12) .
C1A C2A 1.516(16) .
C2A C7A 1.347(14) .
C2A C3A 1.367(13) .
C3A C4A 1.414(13) .
C4A C5A 1.373(13) .
C4A C8A 1.526(12) .
C5A C6A 1.382(13) .
C6A C7A 1.357(14) .
O1MA C1MA 1.63(3) .
Cu2 O1DB 1.78(3) .
Cu2 O1B 1.935(8) .
Cu2 O1WB 1.966(10) .
Cu2 O2WB 2.30(2) .
Cu2 S1DB 2.80(3) .
O1B C1B 1.253(15) .
O2B C1B 1.235(13) .
O3B N1B 1.233(14) .
O4B N1B 1.209(15) .
O5B C8B 1.216(13) .
O6B C8B 1.239(13) .
N1B C6B 1.456(13) .
C1B C2B 1.47(2) 2_645
C2B C3B 1.358(13) .
C2B C7B 1.373(13) .
C2B C1B 1.47(2) 3_765
C3B C4B 1.435(12) .
C4B C5B 1.369(13) .
C4B C8B 1.499(14) .
C5B C6B 1.389(13) .
C6B C7B 1.354(13) .
O1DB S1DB 1.32(2) .
S1DB C2DB 1.89(2) .
S1DB C1DB 1.92(2) .
O1DA S1DA 1.291(14) .
S1DA C1DA 1.87(2) .
S1DA C2DA 1.95(2) .
O1M C1M 1.466(16) .
O2M C2M 1.49(3) .
