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#$Date: 2016-03-24 02:03:07 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179553 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/22/4502212.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_4502212
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 Mo N12 O S3, 0.33(C9 N3 O3), Cl O4'
_chemical_formula_sum            'C36 H48 Cl Cu3 Mo N13 O6 S3'
_chemical_formula_weight         1177.06
_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                   12.8184(18)
_cell_length_b                   12.8184(18)
_cell_length_c                   17.258(4)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.18
_cell_volume                     2455.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24261
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  0.7088
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1193
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.048(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2994
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0291
_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)+(0.0258P)²+1.2946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                2924
_reflns_number_total             2994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9006636_si_002.cif
_cod_data_source_block           '[MoOS3Cu3(dmpzm)3](ClO4).DMF'
_cod_original_sg_symbol_H-M      'P 31c'
_cod_database_code               4502212
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 1.0000 1.0000 0.24142(5) 0.02790(13) Uani 1 3 d S . .
Cu1 Cu 0.85453(5) 0.81308(5) 0.15133(3) 0.03183(13) Uani 1 1 d . . .
S1 S 1.03919(10) 0.85794(10) 0.19448(9) 0.0330(3) Uani 1 1 d . . .
Cl1 Cl 0.3333 0.6667 -0.00834(14) 0.0438(4) Uani 1 3 d S . .
O1 O 1.0000 1.0000 0.3392(3) 0.0485(14) Uani 1 3 d S . .
O3 O 0.3333 0.6667 -0.0897(4) 0.089(3) Uani 1 3 d S . .
O4 O 0.3178(5) 0.5548(5) 0.0179(3) 0.0821(15) Uani 1 1 d . . .
N1 N 0.6180(3) 0.5825(3) 0.1545(3) 0.0387(9) Uani 1 1 d . . .
N2 N 0.7092(3) 0.6547(3) 0.2030(2) 0.0317(9) Uani 1 1 d . . .
N3 N 0.8093(3) 0.7386(3) 0.0438(2) 0.0349(9) Uani 1 1 d . . .
N4 N 0.6920(4) 0.6560(4) 0.0276(2) 0.0443(11) Uani 1 1 d . . .
C1 C 0.4552(5) 0.3696(5) 0.1353(4) 0.074(2) Uani 1 1 d . . .
H1A H 0.3905 0.3888 0.1297 0.111 Uiso 1 1 calc R . .
H1B H 0.4247 0.2932 0.1631 0.111 Uiso 1 1 calc R . .
H1C H 0.4836 0.3627 0.0839 0.111 Uiso 1 1 calc R . .
C2 C 0.5568(4) 0.4673(4) 0.1796(3) 0.0440(13) Uani 1 1 d . . .
C3 C 0.6093(4) 0.4662(4) 0.2483(3) 0.0430(12) Uani 1 1 d . . .
H3 H 0.5862 0.3988 0.2813 0.052 Uiso 1 1 calc R . .
C4 C 0.7036(4) 0.5840(4) 0.2606(3) 0.0336(11) Uani 1 1 d . . .
C5 C 0.7919(5) 0.6333(5) 0.3257(3) 0.0466(13) Uani 1 1 d . . .
H5A H 0.8691 0.6429 0.3087 0.070 Uiso 1 1 calc R . .
H5B H 0.7614 0.5775 0.3697 0.070 Uiso 1 1 calc R . .
H5C H 0.8031 0.7117 0.3414 0.070 Uiso 1 1 calc R . .
C6 C 0.6025(5) 0.6371(5) 0.0848(3) 0.0471(13) Uani 1 1 d . . .
H6A H 0.5211 0.5841 0.0632 0.057 Uiso 1 1 calc R . .
H6B H 0.6089 0.7153 0.0982 0.057 Uiso 1 1 calc R . .
C7 C 0.5602(7) 0.5056(6) -0.0735(4) 0.085(3) Uani 1 1 d . . .
H7A H 0.5347 0.4291 -0.0468 0.128 Uiso 1 1 calc R . .
H7B H 0.5679 0.4954 -0.1291 0.128 Uiso 1 1 calc R . .
H7C H 0.5002 0.5305 -0.0652 0.128 Uiso 1 1 calc R . .
C8 C 0.6801(6) 0.6007(5) -0.0419(3) 0.0563(16) Uani 1 1 d . . .
C9 C 0.7947(6) 0.6506(6) -0.0707(3) 0.0599(18) Uani 1 1 d . . .
H9 H 0.8172 0.6312 -0.1187 0.072 Uiso 1 1 calc R . .
C10 C 0.8720(5) 0.7348(4) -0.0170(3) 0.0430(11) Uani 1 1 d . . .
C11 C 1.0048(5) 0.8137(5) -0.0207(3) 0.0542(15) Uani 1 1 d . . .
H11A H 1.0260 0.8677 -0.0654 0.081 Uiso 1 1 calc R . .
H11B H 1.0427 0.7640 -0.0261 0.081 Uiso 1 1 calc R . .
H11C H 1.0334 0.8615 0.0269 0.081 Uiso 1 1 calc R . .
O2 O 0.6462(19) 0.1745(16) 0.7572(10) 0.107(5) Uani 0.33 1 d PD A -1
N5 N 0.687(3) 0.3516(18) 0.7392(8) 0.107(5) Uani 0.33 1 d PD A -1
C12 C 0.753(3) 0.4784(19) 0.7261(18) 0.107(5) Uani 0.33 1 d PD A -1
C13 C 0.568(3) 0.323(2) 0.7202(19) 0.107(5) Uani 0.33 1 d PD A -1
C14 C 0.732(3) 0.274(2) 0.7448(17) 0.107(5) Uani 0.33 1 d PD A -1
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'
Mo Mo -1.6832 0.6857 '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 Mo1 S1 110.93(4) . 3_675
O1 Mo1 S1 110.93(4) . .
S1 Mo1 S1 107.97(5) 3_675 .
O1 Mo1 S1 110.93(4) . 2_765
S1 Mo1 S1 107.97(5) 3_675 2_765
S1 Mo1 S1 107.97(5) . 2_765
O1 Mo1 Cu1 125.50(2) . .
S1 Mo1 Cu1 54.28(4) 3_675 .
S1 Mo1 Cu1 53.74(4) . .
S1 Mo1 Cu1 123.56(6) 2_765 .
O1 Mo1 Cu1 125.50(2) . 2_765
S1 Mo1 Cu1 123.56(6) 3_675 2_765
S1 Mo1 Cu1 54.28(4) . 2_765
S1 Mo1 Cu1 53.74(4) 2_765 2_765
Cu1 Mo1 Cu1 89.66(3) . 2_765
O1 Mo1 Cu1 125.50(2) . 3_675
S1 Mo1 Cu1 53.74(4) 3_675 3_675
S1 Mo1 Cu1 123.56(6) . 3_675
S1 Mo1 Cu1 54.28(4) 2_765 3_675
Cu1 Mo1 Cu1 89.66(3) . 3_675
Cu1 Mo1 Cu1 89.66(3) 2_765 3_675
N3 Cu1 N2 91.53(14) . .
N3 Cu1 S1 115.84(12) . .
N2 Cu1 S1 113.98(12) . .
N3 Cu1 S1 123.91(12) . 3_675
N2 Cu1 S1 102.08(11) . 3_675
S1 Cu1 S1 107.45(7) . 3_675
N3 Cu1 Mo1 149.01(11) . .
N2 Cu1 Mo1 119.46(10) . .
S1 Cu1 Mo1 53.83(4) . .
S1 Cu1 Mo1 53.67(3) 3_675 .
Cu1 S1 Mo1 72.43(4) . .
Cu1 S1 Cu1 112.17(6) . 2_765
Mo1 S1 Cu1 72.06(4) . 2_765
O3 Cl1 O4 108.6(2) . 3_565
O3 Cl1 O4 108.6(2) . 2_665
O4 Cl1 O4 110.3(2) 3_565 2_665
O3 Cl1 O4 108.6(2) . .
O4 Cl1 O4 110.3(2) 3_565 .
O4 Cl1 O4 110.3(2) 2_665 .
C2 N1 N2 112.2(4) . .
C2 N1 C6 130.3(4) . .
N2 N1 C6 117.4(4) . .
C4 N2 N1 105.3(4) . .
C4 N2 Cu1 133.2(3) . .
N1 N2 Cu1 115.6(3) . .
C10 N3 N4 105.1(4) . .
C10 N3 Cu1 134.2(3) . .
N4 N3 Cu1 119.7(3) . .
C8 N4 N3 112.1(5) . .
C8 N4 C6 130.1(5) . .
N3 N4 C6 117.7(4) . .
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 105.6(4) . .
N1 C2 C1 122.7(4) . .
C3 C2 C1 131.7(5) . .
C2 C3 C4 106.5(4) . .
C2 C3 H3 126.7 . .
C4 C3 H3 126.7 . .
N2 C4 C3 110.3(4) . .
N2 C4 C5 120.4(4) . .
C3 C4 C5 129.3(4) . .
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 . .
N4 C6 N1 111.1(4) . .
N4 C6 H6A 109.4 . .
N1 C6 H6A 109.4 . .
N4 C6 H6B 109.4 . .
N1 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 . .
N4 C8 C9 105.2(5) . .
N4 C8 C7 122.9(7) . .
C9 C8 C7 131.9(6) . .
C8 C9 C10 107.6(5) . .
C8 C9 H9 126.2 . .
C10 C9 H9 126.2 . .
N3 C10 C9 110.0(5) . .
N3 C10 C11 120.9(4) . .
C9 C10 C11 129.0(5) . .
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 . .
C14 N5 C13 128.1(12) . .
C14 N5 C12 127.0(13) . .
C13 N5 C12 102.1(19) . .
O2 C14 N5 106.0(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.687(5) .
Mo1 S1 2.2669(13) 3_675
Mo1 S1 2.2669(13) .
Mo1 S1 2.2669(13) 2_765
Mo1 Cu1 2.6772(8) .
Mo1 Cu1 2.6772(8) 2_765
Mo1 Cu1 2.6772(8) 3_675
Cu1 N3 2.035(4) .
Cu1 N2 2.146(4) .
Cu1 S1 2.2642(13) .
Cu1 S1 2.2846(14) 3_675
S1 Cu1 2.2846(14) 2_765
Cl1 O3 1.405(7) .
Cl1 O4 1.420(5) 3_565
Cl1 O4 1.420(5) 2_665
Cl1 O4 1.420(5) .
N1 C2 1.351(6) .
N1 N2 1.357(6) .
N1 C6 1.454(7) .
N2 C4 1.322(6) .
N3 C10 1.338(6) .
N3 N4 1.367(5) .
N4 C8 1.361(7) .
N4 C6 1.440(7) .
C1 C2 1.489(7) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.367(7) .
C3 C4 1.401(7) .
C3 H3 0.9500 .
C4 C5 1.492(7) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.508(9) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.369(9) .
C9 C10 1.391(8) .
C9 H9 0.9500 .
C10 C11 1.484(8) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
O2 C14 1.214(18) .
N5 C14 1.392(18) .
N5 C13 1.416(13) .
N5 C12 1.426(13) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C6 H6A O4 0.99 2.56 3.451(7) 149.4
