#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/58/4105815.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_4105815
loop_
_publ_author_name
'Zhen-Zhong Lu'
'Rui Zhang'
'Yi-Zhi Li'
'Zi-Jian Guo'
'He-Gen Zheng'
_publ_section_title
;
 Solvatochromic Behavior of a Nanotubular Metal-Organic Framework for
 Sensing Small Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4172
_journal_page_last               4174
_journal_paper_doi               10.1021/ja109437d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C36 H24 Cu4 I2 N18 S4 W'
_chemical_formula_sum            'C36 H24 Cu4 I2 N18 S4 W'
_chemical_formula_weight         1528.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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            8
_cell_length_a                   26.589(7)
_cell_length_b                   31.767(8)
_cell_length_c                   13.739(3)
_cell_measurement_reflns_used    4735
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.11
_cell_volume                     11605(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29583
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    4.666
_exptl_absorpt_correction_T_max  0.326
_exptl_absorpt_correction_T_min  0.227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             5808.0
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.909
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0790P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                4400
_reflns_number_total             5721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109437d_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        11604(5)
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4105815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x, y+1/2, z-1/2'
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
C1 C 0.6955(3) 0.3972(2) 0.6516(5) 0.0313(16) Uani 1 1 d .
H1 H 0.7087 0.4227 0.6303 0.038 Uiso 1 1 calc R
C2 C 0.6994(3) 0.3602(2) 0.5941(6) 0.0354(18) Uani 1 1 d .
H2 H 0.7167 0.3606 0.5353 0.042 Uiso 1 1 calc R
C3 C 0.6777(3) 0.3243(2) 0.6262(6) 0.0353(18) Uani 1 1 d .
C4 C 0.6542(3) 0.3203(2) 0.7147(6) 0.0349(17) Uani 1 1 d .
H4 H 0.6418 0.2944 0.7352 0.042 Uiso 1 1 calc R
C5 C 0.6492(3) 0.3557(2) 0.7727(6) 0.0423(19) Uani 1 1 d .
H5 H 0.6317 0.3540 0.8311 0.051 Uiso 1 1 calc R
C6 C 0.6777(3) 0.2874(3) 0.5645(7) 0.050(2) Uani 1 1 d .
C7 C 0.6880(3) 0.2177(3) 0.4467(6) 0.0417(19) Uani 1 1 d .
C8 C 0.6846(2) 0.1847(2) 0.3816(5) 0.0300(16) Uani 1 1 d .
C9 C 0.7017(3) 0.1873(2) 0.2866(6) 0.0332(17) Uani 1 1 d .
H9 H 0.7135 0.2131 0.2644 0.040 Uiso 1 1 calc R
C10 C 0.7022(3) 0.1542(2) 0.2241(6) 0.0390(19) Uani 1 1 d .
H10 H 0.7143 0.1574 0.1610 0.047 Uiso 1 1 calc R
C11 C 0.6681(3) 0.1112(3) 0.3524(6) 0.0424(19) Uani 1 1 d .
H11 H 0.6572 0.0852 0.3751 0.051 Uiso 1 1 calc R
C12 C 0.6684(3) 0.1452(3) 0.4131(5) 0.0353(18) Uani 1 1 d .
H12 H 0.6575 0.1419 0.4771 0.042 Uiso 1 1 calc R
C13 C 0.6256(3) 0.5404(2) 0.9977(6) 0.0390(19) Uani 1 1 d .
H13 H 0.6435 0.5159 0.9850 0.047 Uiso 1 1 calc R
C14 C 0.5912(3) 0.5428(3) 1.0796(6) 0.045(2) Uani 1 1 d .
H14 H 0.5871 0.5199 1.1208 0.054 Uiso 1 1 calc R
C15 C 0.5659(3) 0.5781(3) 1.0950(6) 0.0409(19) Uani 1 1 d .
C16 C 0.5697(3) 0.6132(2) 1.0323(6) 0.0419(19) Uani 1 1 d .
H16 H 0.5504 0.6371 1.0431 0.050 Uiso 1 1 calc R
C17 C 0.6038(3) 0.6111(2) 0.9517(6) 0.0397(19) Uani 1 1 d .
H17 H 0.6072 0.6338 0.9092 0.048 Uiso 1 1 calc R
C18 C 0.5356(4) 0.5798(3) 1.1778(5) 0.043(2) Uani 1 1 d .
Cu1 Cu 0.67194(4) 0.44530(3) 0.83876(7) 0.0365(2) Uani 1 1 d .
Cu2 Cu 0.68725(3) 0.56627(3) 0.83035(7) 0.0328(2) Uani 1 1 d .
I1 I 0.591016(19) 0.432901(16) 0.93645(3) 0.03664(15) Uani 1 1 d .
N1 N 0.6704(2) 0.39383(16) 0.7436(5) 0.0312(14) Uani 1 1 d .
N2 N 0.6604(2) 0.24994(18) 0.5927(5) 0.0361(15) Uani 1 1 d .
N3 N 0.6658(2) 0.2136(2) 0.5336(5) 0.0432(16) Uani 1 1 d .
N4 N 0.7073(3) 0.2560(2) 0.4138(5) 0.0411(17) Uani 1 1 d .
N5 N 0.7013(3) 0.2919(2) 0.4739(5) 0.0390(15) Uani 1 1 d .
N6 N 0.6844(2) 0.1154(2) 0.2557(5) 0.0420(17) Uani 1 1 d .
N7 N 0.6310(2) 0.57577(19) 0.9386(4) 0.0332(14) Uani 1 1 d .
N8 N 0.5156(3) 0.5432(2) 1.2097(5) 0.0409(16) Uani 1 1 d .
N9 N 0.5161(2) 0.61855(19) 1.2102(4) 0.0350(14) Uani 1 1 d .
S1 S 0.68242(7) 0.50518(6) 0.74546(15) 0.0361(4) Uani 1 1 d .
S2 S 0.75691(6) 0.55754(6) 0.92879(14) 0.0323(4) Uani 1 1 d .
W1 W 0.7500 0.5000 0.83831(3) 0.02767(13) Uani 1 2 d S
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'
S S 0.1246 0.1234 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C2 C1 N1 117.6(6) . .
C2 C1 H1 121.2 . .
N1 C1 H1 121.2 . .
C3 C2 C1 119.0(7) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C2 C3 C4 124.1(7) . .
C2 C3 C6 119.6(8) . .
C4 C3 C6 116.3(7) . .
C3 C4 C5 118.6(7) . .
C3 C4 H4 120.7 . .
C5 C4 H4 120.7 . .
C4 C5 N1 120.2(7) . .
C4 C5 H5 119.9 . .
N1 C5 H5 119.9 . .
N2 C6 N5 120.2(7) . .
N2 C6 C3 123.6(8) . .
N5 C6 C3 115.9(7) . .
N3 C7 C8 118.3(8) . .
N3 C7 N4 122.5(8) . .
C8 C7 N4 118.4(8) . .
C7 C8 C9 122.9(8) . .
C7 C8 C12 120.1(7) . .
C9 C8 C12 116.5(7) . .
C10 C9 C8 123.6(7) . .
C10 C9 H9 118.2 . .
C8 C9 H9 118.2 . .
C9 C10 N6 119.0(7) . .
C9 C10 H10 120.5 . .
N6 C10 H10 120.5 . .
C12 C11 N6 120.1(8) . .
C12 C11 H11 119.9 . .
N6 C11 H11 119.9 . .
C11 C12 C8 121.5(7) . .
C11 C12 H12 119.2 . .
C8 C12 H12 119.2 . .
N7 C13 C14 118.4(7) . .
N7 C13 H13 120.8 . .
C14 C13 H13 120.8 . .
C15 C14 C13 119.2(8) . .
C15 C14 H14 120.4 . .
C13 C14 H14 120.4 . .
C14 C15 C18 117.3(8) . .
C14 C15 C16 122.3(8) . .
C18 C15 C16 120.4(8) . .
C15 C16 C17 118.7(8) . .
C15 C16 H16 120.7 . .
C17 C16 H16 120.7 . .
N7 C17 C16 118.7(6) . .
N7 C17 H17 120.7 . .
C16 C17 H17 120.7 . .
N8 C18 C15 117.2(7) . .
N8 C18 N9 120.3(7) . .
C15 C18 N9 120.4(8) . .
N1 Cu1 S2 109.04(18) . 2_665
N1 Cu1 S1 107.39(18) . .
S2 Cu1 S1 103.61(8) 2_665 .
N1 Cu1 I1 100.98(18) . .
S2 Cu1 I1 114.15(6) 2_665 .
S1 Cu1 I1 121.18(6) . .
N1 Cu1 W1 120.97(18) . .
S2 Cu1 W1 52.09(5) 2_665 .
S1 Cu1 W1 51.52(5) . .
I1 Cu1 W1 137.96(4) . .
N6 Cu2 N7 106.3(3) 14_556 .
N6 Cu2 S1 111.7(2) 14_556 .
N7 Cu2 S1 116.14(18) . .
N6 Cu2 S2 118.7(2) 14_556 .
N7 Cu2 S2 99.85(18) . .
S1 Cu2 S2 104.11(8) . .
N6 Cu2 W1 132.3(2) 14_556 .
N7 Cu2 W1 121.20(16) . .
S1 Cu2 W1 52.12(5) . .
S2 Cu2 W1 52.02(5) . .
C5 N1 C1 120.3(6) . .
C5 N1 Cu1 120.5(5) . .
C1 N1 Cu1 118.9(4) . .
C6 N2 N3 121.7(6) . .
C7 N3 N2 118.4(7) . .
C7 N4 N5 118.1(6) . .
C6 N5 N4 119.1(6) . .
C10 N6 C11 119.1(7) . .
C10 N6 Cu2 120.3(5) . 14_546
C11 N6 Cu2 120.4(6) . 14_546
C17 N7 C13 122.6(6) . .
C17 N7 Cu2 125.9(5) . .
C13 N7 Cu2 111.4(5) . .
C18 N8 N8 119.7(4) . 3_657
N9 N9 C18 118.4(4) 3_657 .
W1 S1 Cu2 73.79(6) . .
W1 S1 Cu1 73.53(6) . .
Cu2 S1 Cu1 115.21(9) . .
W1 S2 Cu1 74.34(7) . 2_665
W1 S2 Cu2 72.80(6) . .
Cu1 S2 Cu2 110.81(9) 2_665 .
S1 W1 S1 109.48(11) . 2_665
S1 W1 S2 109.24(7) . .
S1 W1 S2 108.51(7) 2_665 .
S1 W1 S2 108.51(7) . 2_665
S1 W1 S2 109.24(7) 2_665 2_665
S2 W1 S2 111.84(10) . 2_665
S1 W1 Cu2 54.09(6) . .
S1 W1 Cu2 122.65(6) 2_665 .
S2 W1 Cu2 55.18(5) . .
S2 W1 Cu2 128.07(5) 2_665 .
S1 W1 Cu2 122.65(6) . 2_665
S1 W1 Cu2 54.09(6) 2_665 2_665
S2 W1 Cu2 128.07(5) . 2_665
S2 W1 Cu2 55.18(5) 2_665 2_665
Cu2 W1 Cu2 175.33(4) . 2_665
S1 W1 Cu1 125.24(6) . 2_665
S1 W1 Cu1 54.94(6) 2_665 2_665
S2 W1 Cu1 53.57(5) . 2_665
S2 W1 Cu1 126.25(5) 2_665 2_665
Cu2 W1 Cu1 88.47(3) . 2_665
Cu2 W1 Cu1 91.54(3) 2_665 2_665
S1 W1 Cu1 54.94(6) . .
S1 W1 Cu1 125.24(6) 2_665 .
S2 W1 Cu1 126.25(5) . .
S2 W1 Cu1 53.57(5) 2_665 .
Cu2 W1 Cu1 91.54(3) . .
Cu2 W1 Cu1 88.47(3) 2_665 .
Cu1 W1 Cu1 179.74(4) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.420(10) .
C1 N1 1.432(10) .
C1 H1 0.9300 .
C2 C3 1.352(11) .
C2 H2 0.9300 .
C3 C4 1.373(12) .
C3 C6 1.446(11) .
C4 C5 1.384(10) .
C4 H4 0.9300 .
C5 N1 1.395(9) .
C5 H5 0.9300 .
C6 N2 1.332(11) .
C6 N5 1.403(11) .
C7 N3 1.340(11) .
C7 C8 1.381(11) .
C7 N4 1.393(11) .
C8 C9 1.384(10) .
C8 C12 1.398(11) .
C9 C10 1.359(10) .
C9 H9 0.9300 .
C10 N6 1.388(10) .
C10 H10 0.9300 .
C11 C12 1.363(11) .
C11 N6 1.404(10) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 N7 1.392(9) .
C13 C14 1.452(10) .
C13 H13 0.9300 .
C14 C15 1.323(12) .
C14 H14 0.9300 .
C15 C18 1.395(11) .
C15 C16 1.412(11) .
C16 C17 1.435(12) .
C16 H16 0.9300 .
C17 N7 1.347(10) .
C17 H17 0.9300 .
C18 N8 1.352(11) .
C18 N9 1.407(10) .
Cu1 N1 2.094(6) .
Cu1 S2 2.262(2) 2_665
Cu1 S1 2.311(2) .
Cu1 I1 2.5663(12) .
Cu1 W1 2.7069(11) .
Cu2 N6 1.961(6) 14_556
Cu2 N7 2.131(6) .
Cu2 S1 2.268(2) .
Cu2 S2 2.310(2) .
Cu2 W1 2.6883(10) .
N2 N3 1.418(9) .
N4 N5 1.417(10) .
N6 Cu2 1.961(6) 14_546
N8 N8 1.383(12) 3_657
N9 N9 1.390(12) 3_657
S1 W1 2.2098(19) .
S2 W1 2.218(2) .
S2 Cu1 2.262(2) 2_665
W1 S1 2.2098(19) 2_665
W1 S2 2.218(2) 2_665
W1 Cu2 2.6883(10) 2_665
W1 Cu1 2.7069(11) 2_665
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.001 0.000 1714 836 ' '
2 0.500 0.237 0.265 1714 836 ' '
