#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:03:07 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179553 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/22/4502214.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_4502214
loop_
_publ_author_name
'Zhang, Wen-Hua'
'Liu, Dong'
'Li, Hong-Xi'
'Ren, Zhi-Gang'
'Zhang, Yong'
'Lang, Jian-Ping'
_publ_section_title
;
 How Does a Non-C3-Symmetry Guest Molecule Fit into aC3-Symmetry Host
 Cavity?
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3
_journal_paper_doi               10.1021/cg9006636
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C33 H48 Cu3 N12 O S3 W, Cl O4, 3(H2 O)'
_chemical_formula_sum            'C33 H54 Cl Cu3 N12 O8 S3 W'
_chemical_formula_weight         1252.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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            2
_cell_length_a                   12.8409(18)
_cell_length_b                   12.8409(18)
_cell_length_c                   17.225(3)
_cell_measurement_reflns_used    1059
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.17
_cell_volume                     2459.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27693
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  0.5660
_exptl_absorpt_correction_T_min  0.5043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details '1823 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.152(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0430P)²+4.0294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                3499
_reflns_number_total             3714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9006636_si_002.cif
_cod_data_source_block           '[WOS3Cu3(dmpzm)3](ClO4).3H2O'
_cod_original_sg_symbol_H-M      P31c
_cod_database_code               4502214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
W1 W 1.0000 0.0000 0.07974(6) 0.02677(9) Uani 1 3 d S
Cu1 Cu 1.04176(7) 0.18826(7) -0.01047(5) 0.03264(17) Uani 1 1 d .
S1 S 0.85832(15) 0.03902(15) 0.03393(12) 0.0328(4) Uani 1 1 d .
Cl1 Cl 0.6667 0.3333 0.8273(2) 0.0404(5) Uani 1 3 d S
O1 O 1.0000 0.0000 0.1802(5) 0.047(2) Uani 1 3 d S
O2 O 0.5547(7) 0.3187(7) 0.8555(4) 0.0686(18) Uani 1 1 d .
O3 O 0.6667 0.3333 0.7451(5) 0.076(4) Uani 1 3 d S
O4 O 0.7085(11) 0.2372(12) 0.0711(4) 0.123(4) Uani 1 1 d .
H1W H 0.7258 0.1842 0.0764 0.185 Uiso 1 1 d .
H2W H 0.6350 0.2122 0.0752 0.185 Uiso 1 1 d .
N1 N 1.0545(5) 0.3460(5) 0.0405(3) 0.0311(12) Uani 1 1 d .
N2 N 1.0330(6) 0.4166(5) -0.0080(4) 0.0350(12) Uani 1 1 d .
N3 N 1.0361(6) 0.3449(6) -0.1344(4) 0.0423(15) Uani 1 1 d .
N4 N 1.0711(6) 0.2615(5) -0.1181(4) 0.0351(13) Uani 1 1 d .
C1 C 1.1593(8) 0.3682(7) 0.1635(4) 0.0443(19) Uani 1 1 d .
H1A H 1.0922 0.2901 0.1795 0.066 Uiso 1 1 calc R
H1B H 1.1849 0.4241 0.2074 0.066 Uiso 1 1 calc R
H1C H 1.2266 0.3582 0.1464 0.066 Uiso 1 1 calc R
C2 C 1.1200(6) 0.4171(6) 0.0981(4) 0.0321(15) Uani 1 1 d .
C3 C 1.1428(7) 0.5348(6) 0.0866(5) 0.0429(17) Uani 1 1 d .
H3 H 1.1863 0.6020 0.1198 0.052 Uiso 1 1 calc R
C4 C 1.0883(8) 0.5325(6) 0.0165(4) 0.0428(18) Uani 1 1 d .
C5 C 1.0803(12) 0.6277(9) -0.0271(6) 0.074(4) Uani 1 1 d .
H5A H 1.0009 0.5936 -0.0514 0.111 Uiso 1 1 calc R
H5B H 1.1426 0.6603 -0.0673 0.111 Uiso 1 1 calc R
H5C H 1.0922 0.6922 0.0086 0.111 Uiso 1 1 calc R
C6 C 0.9642(8) 0.3617(8) -0.0770(5) 0.0437(18) Uani 1 1 d .
H6A H 0.9343 0.4133 -0.0987 0.052 Uiso 1 1 calc R
H6B H 0.8937 0.2829 -0.0636 0.052 Uiso 1 1 calc R
C7 C 1.0519(14) 0.4934(11) -0.2349(7) 0.081(4) Uani 1 1 d .
H7A H 1.1118 0.5731 -0.2157 0.122 Uiso 1 1 calc R
H7B H 0.9717 0.4746 -0.2175 0.122 Uiso 1 1 calc R
H7C H 1.0540 0.4929 -0.2918 0.122 Uiso 1 1 calc R
C8 C 1.0800(9) 0.4006(8) -0.2037(5) 0.052(2) Uani 1 1 d .
C9 C 1.1438(9) 0.3514(9) -0.2328(5) 0.055(3) Uani 1 1 d .
H9 H 1.1857 0.3711 -0.2808 0.066 Uiso 1 1 calc R
C10 C 1.1365(8) 0.2666(6) -0.1792(4) 0.0405(15) Uani 1 1 d .
C11 C 1.1918(9) 0.1872(9) -0.1822(7) 0.057(3) Uani 1 1 d .
H11A H 1.1683 0.1361 -0.1359 0.086 Uiso 1 1 calc R
H11B H 1.2796 0.2373 -0.1840 0.086 Uiso 1 1 calc R
H11C H 1.1635 0.1366 -0.2287 0.086 Uiso 1 1 calc 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'
O O 0.0106 0.0060 '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'
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'
W W -0.8490 6.8722 '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
O1 W1 S1 110.46(6) . .
O1 W1 S1 110.46(6) . 3_765
S1 W1 S1 108.46(6) . 3_765
O1 W1 S1 110.46(6) . 2_645
S1 W1 S1 108.46(6) . 2_645
S1 W1 S1 108.46(6) 3_765 2_645
O1 W1 Cu1 125.25(3) . 2_645
S1 W1 Cu1 53.96(5) . 2_645
S1 W1 Cu1 124.29(8) 3_765 2_645
S1 W1 Cu1 54.53(5) 2_645 2_645
O1 W1 Cu1 125.25(3) . 3_765
S1 W1 Cu1 124.29(8) . 3_765
S1 W1 Cu1 54.53(5) 3_765 3_765
S1 W1 Cu1 53.96(5) 2_645 3_765
Cu1 W1 Cu1 90.03(4) 2_645 3_765
O1 W1 Cu1 125.25(3) . .
S1 W1 Cu1 54.53(5) . .
S1 W1 Cu1 53.96(5) 3_765 .
S1 W1 Cu1 124.29(8) 2_645 .
Cu1 W1 Cu1 90.03(4) 2_645 .
Cu1 W1 Cu1 90.03(4) 3_765 .
N4 Cu1 N1 91.6(2) . .
N4 Cu1 S1 116.12(19) . 3_765
N1 Cu1 S1 114.34(17) . 3_765
N4 Cu1 S1 124.47(19) . .
N1 Cu1 S1 102.36(17) . .
S1 Cu1 S1 106.25(9) 3_765 .
N4 Cu1 W1 148.38(16) . .
N1 Cu1 W1 120.02(15) . .
S1 Cu1 W1 53.22(5) 3_765 .
S1 Cu1 W1 53.05(5) . .
W1 S1 Cu1 72.82(6) . 2_645
W1 S1 Cu1 72.41(6) . .
Cu1 S1 Cu1 112.55(9) 2_645 .
O3 Cl1 O2 109.7(3) . 2_655
O3 Cl1 O2 109.7(3) . 3_665
O2 Cl1 O2 109.2(3) 2_655 3_665
O3 Cl1 O2 109.7(3) . .
O2 Cl1 O2 109.2(3) 2_655 .
O2 Cl1 O2 109.2(3) 3_665 .
H1W O4 H2W 113.2 . .
C2 N1 N2 105.8(5) . .
C2 N1 Cu1 132.9(5) . .
N2 N1 Cu1 115.8(4) . .
C4 N2 N1 111.8(6) . .
C4 N2 C6 130.6(6) . .
N1 N2 C6 117.5(6) . .
C8 N3 N4 112.1(7) . .
C8 N3 C6 130.7(7) . .
N4 N3 C6 117.3(6) . .
C10 N4 N3 104.1(6) . .
C10 N4 Cu1 135.6(5) . .
N3 N4 Cu1 119.2(5) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 C3 110.7(6) . .
N1 C2 C1 120.4(6) . .
C3 C2 C1 128.9(6) . .
C4 C3 C2 105.6(6) . .
C4 C3 H3 127.2 . .
C2 C3 H3 127.2 . .
N2 C4 C3 106.0(6) . .
N2 C4 C5 122.2(7) . .
C3 C4 C5 131.7(7) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N2 C6 N3 111.0(6) . .
N2 C6 H6A 109.4 . .
N3 C6 H6A 109.4 . .
N2 C6 H6B 109.4 . .
N3 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
C8 C7 H7A 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C8 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 N3 105.5(8) . .
C9 C8 C7 132.6(9) . .
N3 C8 C7 121.9(10) . .
C8 C9 C10 107.5(8) . .
C8 C9 H9 126.3 . .
C10 C9 H9 126.3 . .
N4 C10 C9 110.9(8) . .
N4 C10 C11 119.6(7) . .
C9 C10 C11 129.4(8) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.730(9) .
W1 S1 2.2572(18) .
W1 S1 2.2572(18) 3_765
W1 S1 2.2572(18) 2_645
W1 Cu1 2.6925(11) 2_645
W1 Cu1 2.6925(11) 3_765
W1 Cu1 2.6925(11) .
Cu1 N4 2.028(6) .
Cu1 N1 2.138(5) .
Cu1 S1 2.279(2) 3_765
Cu1 S1 2.300(2) .
S1 Cu1 2.279(2) 2_645
Cl1 O3 1.416(10) .
Cl1 O2 1.438(7) 2_655
Cl1 O2 1.438(7) 3_665
Cl1 O2 1.438(7) .
O4 H1W 0.820 .
O4 H2W 0.834 .
N1 C2 1.326(9) .
N1 N2 1.358(8) .
N2 C4 1.357(9) .
N2 C6 1.438(10) .
N3 C8 1.361(10) .
N3 N4 1.382(8) .
N3 C6 1.441(11) .
N4 C10 1.327(10) .
C1 C2 1.494(10) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.404(10) .
C3 C4 1.387(11) .
C3 H3 0.9500 .
C4 C5 1.481(11) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.505(14) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.356(14) .
C9 C10 1.394(11) .
C9 H9 0.9500 .
C10 C11 1.507(12) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
