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#$Date: 2025-08-20 17:12:52 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/48/4104839.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_4104839
loop_
_publ_author_name
'C. W. Liu'
'Bijay Sarkar'
'Yao-Jheng Huang'
'Ping-Kuei Liao'
'Ju-Chun Wang'
'Jean-Yves Saillard'
'Samia Kahlal'
_publ_section_title
;
 Octanuclear Copper(I) Clusters Inscribed in a Se12 Icosahedron:
 Anion-Induced Modulation of the Core Size and Symmetry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11222
_journal_page_last               11233
_journal_paper_doi               10.1021/ja904089t
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C36 H84 Cu8 F12 O12 P8 Se12'
_chemical_formula_weight         2640.63
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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            1
_cell_length_a                   14.7070(2)
_cell_length_b                   14.7070(2)
_cell_length_c                   10.8676(3)
_cell_measurement_reflns_used    2234
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.64
_cell_measurement_theta_min      2.46
_cell_volume                     2035.69(7)
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13653
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    7.639
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.871
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0410
_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)+(0.0643P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                2209
_reflns_number_total             3374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja904089t_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4104839
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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
Se1 Se 0.18398(4) 1.09941(4) 0.78054(5) 0.04620(16) Uani 1 1 d .
Se2 Se 0.11147(4) 1.28669(4) 0.57344(5) 0.04645(17) Uani 1 1 d .
Cu1 Cu 0.0000 1.0000 0.76611(12) 0.0548(3) Uani 1 3 d S
Cu2 Cu 0.17877(5) 1.17154(5) 0.58847(6) 0.0542(2) Uani 1 1 d .
P1 P 0.23035(9) 0.98228(10) 0.74245(12) 0.0416(3) Uani 1 1 d .
P2 P 0.3333 0.6667 0.6603(3) 0.0656(7) Uani 1 3 d S
O1 O 0.1898(3) 0.9076(3) 0.8564(3) 0.0520(9) Uani 1 1 d .
O2 O 0.3507(3) 1.0314(3) 0.7536(4) 0.0561(9) Uani 1 1 d .
C1 C 0.2114(4) 0.8201(4) 0.8685(5) 0.0524(13) Uani 1 1 d .
H1 H 0.2396 0.8107 0.7908 0.063 Uiso 1 1 calc R
C2 C 0.1079(5) 0.7235(5) 0.8957(8) 0.084(2) Uani 1 1 d .
H2A H 0.0757 0.7365 0.9652 0.126 Uiso 1 1 calc R
H2B H 0.1192 0.6660 0.9139 0.126 Uiso 1 1 calc R
H2C H 0.0627 0.7062 0.8254 0.126 Uiso 1 1 calc R
C3 C 0.2915(6) 0.8479(6) 0.9694(6) 0.082(2) Uani 1 1 d .
H3A H 0.3538 0.9127 0.9494 0.123 Uiso 1 1 calc R
H3B H 0.3085 0.7931 0.9774 0.123 Uiso 1 1 calc R
H3C H 0.2631 0.8557 1.0457 0.123 Uiso 1 1 calc R
C4 C 0.4332(4) 1.0908(5) 0.6613(6) 0.0656(16) Uani 1 1 d .
H4 H 0.4020 1.0802 0.5791 0.079 Uiso 1 1 calc R
C5 C 0.4842(6) 1.2039(5) 0.6963(9) 0.108(3) Uani 1 1 d .
H5A H 0.4314 1.2202 0.7218 0.162 Uiso 1 1 calc R
H5B H 0.5216 1.2466 0.6269 0.162 Uiso 1 1 calc R
H5C H 0.5323 1.2176 0.7629 0.162 Uiso 1 1 calc R
C6 C 0.5051(7) 1.0494(7) 0.6658(10) 0.126(4) Uani 1 1 d .
H6A H 0.5312 1.0553 0.7481 0.190 Uiso 1 1 calc R
H6B H 0.5628 1.0887 0.6107 0.190 Uiso 1 1 calc R
H6C H 0.4686 0.9769 0.6415 0.190 Uiso 1 1 calc R
F1 F 0.3893(7) 0.7636(7) 0.7352(11) 0.244(5) Uani 1 1 d .
F2 F 0.4310(8) 0.7054(9) 0.5897(11) 0.298(6) Uani 1 1 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
P1 Se1 Cu1 102.29(4) . .
P1 Se1 Cu2 106.25(4) . .
Cu1 Se1 Cu2 86.25(4) . .
P1 Se2 Cu2 109.78(4) 2_675 6_666
P1 Se2 Cu2 101.04(4) 2_675 .
Cu2 Se2 Cu2 86.17(3) 6_666 .
Se1 Cu1 Se1 119.561(8) 3_465 .
Se1 Cu1 Se1 119.558(8) 3_465 2_675
Se1 Cu1 Se1 119.559(8) . 2_675
Se2 Cu2 Se2 116.92(3) 5_456 .
Se2 Cu2 Se1 119.93(3) 5_456 .
Se2 Cu2 Se1 120.28(3) . .
O2 P1 O1 102.2(2) . .
O2 P1 Se1 110.64(16) . .
O1 P1 Se1 104.14(14) . .
O2 P1 Se2 109.64(16) . 3_465
O1 P1 Se2 109.29(15) . 3_465
Se1 P1 Se2 119.39(6) . 3_465
F2 P2 F2 95.2(8) 3_565 .
F2 P2 F2 95.2(8) 3_565 2_665
F2 P2 F2 95.2(8) . 2_665
F2 P2 F1 87.1(6) 3_565 3_565
F2 P2 F1 85.0(6) . 3_565
F2 P2 F1 177.6(7) 2_665 3_565
F2 P2 F1 177.6(7) 3_565 .
F2 P2 F1 87.1(6) . .
F2 P2 F1 85.0(6) 2_665 .
F1 P2 F1 92.7(7) 3_565 .
F2 P2 F1 85.0(6) 3_565 2_665
F2 P2 F1 177.6(7) . 2_665
F2 P2 F1 87.1(6) 2_665 2_665
F1 P2 F1 92.7(7) 3_565 2_665
F1 P2 F1 92.7(7) . 2_665
C1 O1 P1 120.7(3) . .
C4 O2 P1 129.3(4) . .
O1 C1 C2 106.4(4) . .
O1 C1 C3 107.9(5) . .
C2 C1 C3 113.4(5) . .
C6 C4 O2 106.4(6) . .
C6 C4 C5 113.0(7) . .
O2 C4 C5 107.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 P1 2.1861(13) .
Se1 Cu1 2.3510(5) .
Se1 Cu2 2.3600(9) .
Se2 P1 2.1941(14) 2_675
Se2 Cu2 2.3520(9) 6_666
Se2 Cu2 2.3560(8) .
Cu1 Se1 2.3509(5) 3_465
Cu1 Se1 2.3511(5) 2_675
Cu2 Se2 2.3520(9) 5_456
P1 O2 1.546(4) .
P1 O1 1.562(4) .
P1 Se2 2.1941(14) 3_465
P2 F2 1.468(6) 3_565
P2 F2 1.468(6) .
P2 F2 1.469(6) 2_665
P2 F1 1.483(6) 3_565
P2 F1 1.483(7) .
P2 F1 1.483(7) 2_665
O1 C1 1.478(6) .
O2 C4 1.477(7) .
C1 C2 1.503(8) .
C1 C3 1.508(8) .
C4 C6 1.461(10) .
C4 C5 1.493(10) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139115626
