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#$Date: 2025-08-21 03:19:08 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301842 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/22/4502209.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_4502209
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, Cl O4 '
_chemical_formula_sum            'C33 H48 Cl Cu3 Mo N12 O5 S3'
_chemical_formula_weight         1111.02
_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                   12.8832(18)
_cell_length_b                   12.8832(18)
_cell_length_c                   17.084(3)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     2455.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24137
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.5413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details '1428 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.014(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2934
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0286
_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)+(0.0646P)²+0.2590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                2911
_reflns_number_total             2934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg9006636_si_002.cif
_cod_data_source_block           '[MoOS3Cu3(dmpzm)3](ClO4)'
_cod_original_sg_symbol_H-M      P31c
_cod_database_code               4502209
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
Mo1 Mo 1.0000 1.0000 0.57880(5) 0.02846(15) Uani 1 3 d S
Cu1 Cu 0.85510(5) 0.81400(4) 0.48824(3) 0.03061(15) Uani 1 1 d .
S1 S 1.03854(10) 0.85860(10) 0.53161(9) 0.0324(3) Uani 1 1 d .
Cl1 Cl 0.3333 0.6667 0.33012(13) 0.0384(4) Uani 1 3 d S
O1 O 1.0000 1.0000 0.6775(4) 0.0575(18) Uani 1 3 d S
O2 O 0.3333 0.6667 0.2467(4) 0.062(2) Uani 1 3 d S
O3 O 0.4447(5) 0.7629(5) 0.3579(3) 0.0678(12) Uani 1 1 d .
N1 N 0.6169(4) 0.5865(4) 0.4921(3) 0.0365(8) Uani 1 1 d .
N2 N 0.7107(3) 0.6555(3) 0.5391(2) 0.0332(9) Uani 1 1 d .
N3 N 0.8072(3) 0.7403(4) 0.3797(3) 0.0359(9) Uani 1 1 d .
N4 N 0.6892(4) 0.6615(4) 0.3642(3) 0.0442(11) Uani 1 1 d .
C1 C 0.4513(6) 0.3750(6) 0.4712(4) 0.071(2) Uani 1 1 d .
H1A H 0.3872 0.3949 0.4705 0.107 Uiso 1 1 calc R
H1B H 0.4227 0.2978 0.4975 0.107 Uiso 1 1 calc R
H1C H 0.4747 0.3698 0.4174 0.107 Uiso 1 1 calc R
C2 C 0.5568(5) 0.4700(5) 0.5142(3) 0.0422(13) Uani 1 1 d .
C3 C 0.6108(4) 0.4659(5) 0.5836(3) 0.0425(12) Uani 1 1 d .
H3 H 0.5877 0.3978 0.6160 0.051 Uiso 1 1 calc R
C4 C 0.7068(4) 0.5831(4) 0.5964(3) 0.0337(10) Uani 1 1 d .
C5 C 0.7965(5) 0.6288(5) 0.6603(3) 0.0397(11) Uani 1 1 d .
H5A H 0.8750 0.6482 0.6394 0.060 Uiso 1 1 calc R
H5B H 0.7724 0.5673 0.7010 0.060 Uiso 1 1 calc R
H5C H 0.8012 0.7010 0.6828 0.060 Uiso 1 1 calc R
C6 C 0.6022(5) 0.6428(5) 0.4231(4) 0.0466(13) Uani 1 1 d .
H6A H 0.5207 0.5916 0.4016 0.056 Uiso 1 1 calc R
H6B H 0.6102 0.7208 0.4378 0.056 Uiso 1 1 calc R
C7 C 0.5535(8) 0.5174(8) 0.2617(5) 0.095(3) Uani 1 1 d .
H7A H 0.5207 0.4437 0.2928 0.143 Uiso 1 1 calc R
H7B H 0.5620 0.4995 0.2071 0.143 Uiso 1 1 calc R
H7C H 0.4992 0.5499 0.2644 0.143 Uiso 1 1 calc R
C8 C 0.6739(6) 0.6077(6) 0.2935(4) 0.0624(19) Uani 1 1 d .
C9 C 0.7893(8) 0.6543(7) 0.2623(4) 0.069(2) Uani 1 1 d .
H9 H 0.8102 0.6349 0.2133 0.083 Uiso 1 1 calc R
C10 C 0.8675(5) 0.7348(4) 0.3179(3) 0.0414(12) Uani 1 1 d .
C11 C 1.0012(6) 0.8110(6) 0.3129(4) 0.0521(16) Uani 1 1 d .
H11A H 1.0226 0.8654 0.2681 0.078 Uiso 1 1 calc R
H11B H 1.0365 0.7596 0.3063 0.078 Uiso 1 1 calc R
H11C H 1.0318 0.8579 0.3611 0.078 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'
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'
Cl Cl 0.1484 0.1585 '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 110.87(5) . 3_675
O1 Mo1 S1 110.87(5) . 2_765
S1 Mo1 S1 108.03(5) 3_675 2_765
O1 Mo1 S1 110.87(5) . .
S1 Mo1 S1 108.03(5) 3_675 .
S1 Mo1 S1 108.03(5) 2_765 .
O1 Mo1 Cu1 125.36(2) . .
S1 Mo1 Cu1 54.37(4) 3_675 .
S1 Mo1 Cu1 123.77(6) 2_765 .
S1 Mo1 Cu1 53.71(4) . .
O1 Mo1 Cu1 125.36(2) . 3_675
S1 Mo1 Cu1 53.71(4) 3_675 3_675
S1 Mo1 Cu1 54.37(4) 2_765 3_675
S1 Mo1 Cu1 123.77(6) . 3_675
Cu1 Mo1 Cu1 89.87(3) . 3_675
O1 Mo1 Cu1 125.36(2) . 2_765
S1 Mo1 Cu1 123.77(6) 3_675 2_765
S1 Mo1 Cu1 53.71(4) 2_765 2_765
S1 Mo1 Cu1 54.37(4) . 2_765
Cu1 Mo1 Cu1 89.87(3) . 2_765
Cu1 Mo1 Cu1 89.87(3) 3_675 2_765
N3 Cu1 N2 90.53(16) . .
N3 Cu1 S1 116.90(12) . .
N2 Cu1 S1 114.12(12) . .
N3 Cu1 S1 122.94(13) . 3_675
N2 Cu1 S1 102.86(12) . 3_675
S1 Cu1 S1 107.37(7) . 3_675
N3 Cu1 Mo1 149.20(12) . .
N2 Cu1 Mo1 120.26(11) . .
S1 Cu1 Mo1 53.81(3) . .
S1 Cu1 Mo1 53.61(3) 3_675 .
Cu1 S1 Mo1 72.48(4) . .
Cu1 S1 Cu1 112.41(6) . 2_765
Mo1 S1 Cu1 72.02(4) . 2_765
O2 Cl1 O3 109.4(2) . 2_665
O2 Cl1 O3 109.4(2) . .
O3 Cl1 O3 109.6(2) 2_665 .
O2 Cl1 O3 109.4(2) . 3_565
O3 Cl1 O3 109.6(2) 2_665 3_565
O3 Cl1 O3 109.6(2) . 3_565
C2 N1 N2 113.1(4) . .
C2 N1 C6 129.6(4) . .
N2 N1 C6 117.0(4) . .
C4 N2 N1 105.5(4) . .
C4 N2 Cu1 132.4(3) . .
N1 N2 Cu1 116.8(3) . .
C10 N3 N4 105.6(4) . .
C10 N3 Cu1 134.3(3) . .
N4 N3 Cu1 119.2(3) . .
C8 N4 N3 112.0(5) . .
C8 N4 C6 129.6(5) . .
N3 N4 C6 118.4(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 105.1(4) . .
N1 C2 C1 123.7(4) . .
C3 C2 C1 131.1(5) . .
C4 C3 C2 106.2(5) . .
C4 C3 H3 126.9 . .
C2 C3 H3 126.9 . .
N2 C4 C3 110.0(5) . .
N2 C4 C5 120.9(4) . .
C3 C4 C5 129.1(5) . .
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 111.7(4) . .
N4 C6 H6A 109.3 . .
N1 C6 H6A 109.3 . .
N4 C6 H6B 109.3 . .
N1 C6 H6B 109.3 . .
H6A C6 H6B 107.9 . .
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 C7 123.2(8) . .
N4 C8 C9 105.5(6) . .
C7 C8 C9 131.2(8) . .
C10 C9 C8 106.1(6) . .
C10 C9 H9 127.0 . .
C8 C9 H9 127.0 . .
N3 C10 C9 110.8(6) . .
N3 C10 C11 121.2(4) . .
C9 C10 C11 127.9(6) . .
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
Mo1 O1 1.686(7) .
Mo1 S1 2.2627(13) 3_675
Mo1 S1 2.2627(13) 2_765
Mo1 S1 2.2627(13) .
Mo1 Cu1 2.6735(8) .
Mo1 Cu1 2.6735(8) 3_675
Mo1 Cu1 2.6735(8) 2_765
Cu1 N3 2.034(4) .
Cu1 N2 2.142(4) .
Cu1 S1 2.2597(13) .
Cu1 S1 2.2846(13) 3_675
S1 Cu1 2.2846(13) 2_765
Cl1 O2 1.425(7) .
Cl1 O3 1.429(5) 2_665
Cl1 O3 1.429(5) .
Cl1 O3 1.429(5) 3_565
N1 C2 1.353(7) .
N1 N2 1.350(6) .
N1 C6 1.445(7) .
N2 C4 1.335(6) .
N3 C10 1.334(7) .
N3 N4 1.367(6) .
N4 C8 1.358(8) .
N4 C6 1.434(8) .
C1 C2 1.491(7) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.389(7) .
C3 C4 1.411(7) .
C3 H3 0.9500 .
C4 C5 1.481(7) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.500(10) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.401(11) .
C9 C10 1.395(9) .
C9 H9 0.9500 .
C10 C11 1.499(9) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
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
_geom_hbond_site_symmetry_A
C6 H6A O3 0.99 2.52 3.431(7) 152.5 3_565
C11 H11A O1 0.98 2.45 3.364(9) 155.5 4_554
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139144889
