#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:08:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179777 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/73/7007334.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_7007334
loop_
_publ_author_name
'Shi, Weifeng'
'Shafaei-Fallah, Maryam'
'Anson, Christopher E.'
'Rothenberger, Alexander'
_publ_section_title
;
 Metal thiophosphonates and related compounds: an emerging area of
 supramolecular coordination chemistry.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3257
_journal_page_last               3262
_journal_paper_doi               10.1039/b603764j
_journal_year                    2006
_chemical_formula_sum            'C80 H78 Cu4 O2 P6 S6'
_chemical_formula_weight         1703.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.538(7)
_cell_angle_beta                 101.470(7)
_cell_angle_gamma                109.779(6)
_cell_formula_units_Z            1
_cell_length_a                   11.8442(10)
_cell_length_b                   13.4796(12)
_cell_length_c                   13.6857(12)
_cell_measurement_reflns_used    14268
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1.6
_cell_volume                     1928.5(3)
_computing_cell_refinement       'stoe winexpose'
_computing_data_collection       'stoe winexpose'
_computing_data_reduction        'stoe winexpose'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'stoe ipds 2'
_diffrn_measurement_method       'area detector'
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16967
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.421
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.491
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0596P)²+1.1404P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                6235
_reflns_number_total             8709
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603764j.txt
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7007334
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.1968(3) 0.3203(3) 0.1508(3) 0.0438(8) Uani 1 1 d . . .
Cu1 Cu 0.02607(6) 0.67255(4) 0.10596(4) 0.03549(14) Uani 1 1 d . . .
Cu2 Cu 0.14442(5) 0.54135(4) 0.15966(4) 0.02954(12) Uani 1 1 d . . .
P1 P -0.12062(10) 0.38067(9) 0.08132(8) 0.0264(2) Uani 1 1 d . . .
P2 P 0.03201(10) 0.82810(8) 0.20540(7) 0.0262(2) Uani 1 1 d . . .
P3 P 0.28862(9) 0.54175(8) 0.29437(7) 0.02393(19) Uani 1 1 d . . .
S1 S -0.05958(10) 0.53667(9) 0.17747(7) 0.0299(2) Uani 1 1 d . . .
S2 S 0.03075(9) 0.34355(8) 0.07091(7) 0.02493(19) Uani 1 1 d . . .
S3 S 0.23393(10) 0.65312(9) 0.06381(8) 0.0326(2) Uani 1 1 d . . .
C1 C -0.2558(5) 0.2081(4) 0.1540(4) 0.0419(11) Uani 1 1 d . . .
C2 C -0.3685(7) 0.1468(6) 0.0521(5) 0.0683(17) Uani 1 1 d . . .
H2A H -0.4250 0.1858 0.0489 0.102 Uiso 1 1 calc R . .
H2B H -0.4142 0.0713 0.0525 0.102 Uiso 1 1 calc R . .
H2C H -0.3367 0.1452 -0.0088 0.102 Uiso 1 1 calc R . .
C3 C -0.1638(7) 0.1539(6) 0.1644(6) 0.072(2) Uani 1 1 d . . .
H3A H -0.0960 0.1950 0.2294 0.108 Uiso 1 1 calc R . .
H3B H -0.1289 0.1534 0.1052 0.108 Uiso 1 1 calc R . .
H3C H -0.2066 0.0781 0.1655 0.108 Uiso 1 1 calc R . .
C4 C -0.3088(6) 0.2174(5) 0.2437(5) 0.0575(15) Uani 1 1 d . . .
H4A H -0.2403 0.2553 0.3087 0.086 Uiso 1 1 calc R . .
H4B H -0.3593 0.1436 0.2453 0.086 Uiso 1 1 calc R . .
H4C H -0.3616 0.2594 0.2361 0.086 Uiso 1 1 calc R . .
C5 C 0.1185(4) 0.9573(3) 0.1796(3) 0.0293(8) Uani 1 1 d . . .
C6 C 0.2302(5) 0.9642(4) 0.1572(4) 0.0390(10) Uani 1 1 d . . .
H6A H 0.2526 0.9024 0.1498 0.047 Uiso 1 1 calc R . .
C7 C 0.3096(5) 1.0630(5) 0.1456(4) 0.0499(12) Uani 1 1 d . . .
H7A H 0.3865 1.0685 0.1315 0.060 Uiso 1 1 calc R . .
C8 C 0.2757(5) 1.1515(4) 0.1547(4) 0.0463(12) Uani 1 1 d . . .
H8A H 0.3297 1.2183 0.1474 0.056 Uiso 1 1 calc R . .
C9 C 0.1631(5) 1.1439(4) 0.1746(4) 0.0446(11) Uani 1 1 d . . .
H9A H 0.1387 1.2045 0.1785 0.053 Uiso 1 1 calc R . .
C10 C 0.0861(5) 1.0472(4) 0.1888(3) 0.0371(9) Uani 1 1 d . . .
H10A H 0.0106 1.0430 0.2049 0.044 Uiso 1 1 calc R . .
C11 C -0.1286(4) 0.8203(3) 0.1900(3) 0.0284(8) Uani 1 1 d . . .
C12 C -0.1897(4) 0.8487(4) 0.1090(4) 0.0414(10) Uani 1 1 d . . .
H12A H -0.1464 0.8775 0.0629 0.050 Uiso 1 1 calc R . .
C13 C -0.3141(5) 0.8351(5) 0.0955(4) 0.0466(11) Uani 1 1 d . . .
H13A H -0.3543 0.8570 0.0415 0.056 Uiso 1 1 calc R . .
C14 C -0.3806(5) 0.7900(4) 0.1597(4) 0.0431(11) Uani 1 1 d . . .
H14A H -0.4656 0.7809 0.1499 0.052 Uiso 1 1 calc R . .
C15 C -0.3214(5) 0.7585(4) 0.2379(4) 0.0439(11) Uani 1 1 d . . .
H15A H -0.3663 0.7265 0.2817 0.053 Uiso 1 1 calc R . .
C16 C -0.1958(5) 0.7734(4) 0.2534(3) 0.0368(10) Uani 1 1 d . . .
H16A H -0.1560 0.7513 0.3075 0.044 Uiso 1 1 calc R . .
C17 C 0.0974(4) 0.8642(3) 0.3472(3) 0.0266(7) Uani 1 1 d . . .
C18 C 0.0988(5) 0.9578(4) 0.4143(3) 0.0352(9) Uani 1 1 d . . .
H18A H 0.0621 1.0029 0.3871 0.042 Uiso 1 1 calc R . .
C19 C 0.1535(5) 0.9848(4) 0.5204(3) 0.0414(10) Uani 1 1 d . . .
H19A H 0.1535 1.0481 0.5658 0.050 Uiso 1 1 calc R . .
C20 C 0.2082(4) 0.9203(4) 0.5608(3) 0.0393(10) Uani 1 1 d . . .
H20A H 0.2459 0.9393 0.6337 0.047 Uiso 1 1 calc R . .
C21 C 0.2077(4) 0.8282(4) 0.4950(3) 0.0372(10) Uani 1 1 d . . .
H21A H 0.2454 0.7839 0.5226 0.045 Uiso 1 1 calc R . .
C22 C 0.1525(4) 0.7999(4) 0.3885(3) 0.0325(9) Uani 1 1 d . . .
H22A H 0.1523 0.7362 0.3436 0.039 Uiso 1 1 calc R . .
C23 C 0.3876(4) 0.6703(4) 0.3969(3) 0.0300(8) Uani 1 1 d . . .
C24 C 0.4278(5) 0.7664(4) 0.3665(4) 0.0392(10) Uani 1 1 d . . .
H24A H 0.3994 0.7640 0.2957 0.047 Uiso 1 1 calc R . .
C25 C 0.5100(5) 0.8658(4) 0.4402(5) 0.0532(14) Uani 1 1 d . . .
H25A H 0.5381 0.9308 0.4192 0.064 Uiso 1 1 calc R . .
C26 C 0.5506(5) 0.8704(5) 0.5431(5) 0.0578(15) Uani 1 1 d . . .
H26A H 0.6071 0.9385 0.5925 0.069 Uiso 1 1 calc R . .
C27 C 0.5100(5) 0.7774(5) 0.5751(4) 0.0539(15) Uani 1 1 d . . .
H27A H 0.5377 0.7815 0.6464 0.065 Uiso 1 1 calc R . .
C28 C 0.4279(4) 0.6763(4) 0.5025(3) 0.0391(10) Uani 1 1 d . . .
H28A H 0.3996 0.6121 0.5246 0.047 Uiso 1 1 calc R . .
C29 C 0.2241(4) 0.4475(3) 0.3671(3) 0.0297(8) Uani 1 1 d . . .
C30 C 0.2677(4) 0.3687(4) 0.3898(3) 0.0348(9) Uani 1 1 d . . .
H30A H 0.3374 0.3631 0.3684 0.042 Uiso 1 1 calc R . .
C31 C 0.2109(5) 0.2973(4) 0.4435(4) 0.0435(11) Uani 1 1 d . . .
H31A H 0.2413 0.2433 0.4579 0.052 Uiso 1 1 calc R . .
C32 C 0.1104(5) 0.3059(5) 0.4755(4) 0.0494(12) Uani 1 1 d . . .
H32A H 0.0729 0.2593 0.5138 0.059 Uiso 1 1 calc R . .
C33 C 0.0640(5) 0.3825(5) 0.4519(5) 0.0573(15) Uani 1 1 d . . .
H33A H -0.0060 0.3873 0.4732 0.069 Uiso 1 1 calc R . .
C34 C 0.1193(5) 0.4523(5) 0.3972(5) 0.0517(14) Uani 1 1 d . . .
H34A H 0.0857 0.5035 0.3801 0.062 Uiso 1 1 calc R . .
C35 C 0.4064(4) 0.4997(3) 0.2500(3) 0.0275(8) Uani 1 1 d . . .
C36 C 0.5185(4) 0.5132(4) 0.3181(4) 0.0369(9) Uani 1 1 d . . .
H36A H 0.5339 0.5410 0.3911 0.044 Uiso 1 1 calc R . .
C37 C 0.6085(5) 0.4861(5) 0.2799(5) 0.0481(12) Uani 1 1 d . . .
H37A H 0.6843 0.4946 0.3268 0.058 Uiso 1 1 calc R . .
C38 C 0.5867(5) 0.4465(4) 0.1729(4) 0.0457(12) Uani 1 1 d . . .
H38A H 0.6482 0.4289 0.1467 0.055 Uiso 1 1 calc R . .
C39 C 0.4762(5) 0.4328(4) 0.1051(4) 0.0418(11) Uani 1 1 d . . .
H39A H 0.4617 0.4053 0.0322 0.050 Uiso 1 1 calc R . .
C40 C 0.3851(4) 0.4590(3) 0.1424(3) 0.0320(9) Uani 1 1 d . . .
H40A H 0.3090 0.4492 0.0951 0.038 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'
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'
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'
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
_geom_angle_publ_flag
C1 O1 P1 136.9(3) . . ?
P2 Cu1 S1 106.78(4) . . ?
P2 Cu1 S2 112.97(4) . 2_565 ?
S1 Cu1 S2 124.25(4) . 2_565 ?
P2 Cu1 S3 122.34(5) . . ?
S1 Cu1 S3 107.86(4) . . ?
S2 Cu1 S3 82.06(3) 2_565 . ?
P2 Cu1 Cu2 128.46(4) . . ?
S1 Cu1 Cu2 58.02(3) . . ?
S2 Cu1 Cu2 115.14(3) 2_565 . ?
S3 Cu1 Cu2 50.41(3) . . ?
P3 Cu2 S3 112.20(4) . . ?
P3 Cu2 S2 101.71(4) . . ?
S3 Cu2 S2 117.60(4) . . ?
P3 Cu2 S1 120.59(4) . . ?
S3 Cu2 S1 115.95(4) . . ?
S2 Cu2 S1 85.12(4) . . ?
P3 Cu2 Cu1 139.36(4) . . ?
S3 Cu2 Cu1 64.72(3) . . ?
S2 Cu2 Cu1 115.64(3) . . ?
S1 Cu2 Cu1 51.89(3) . . ?
O1 P1 S3 110.95(15) . 2_565 ?
O1 P1 S1 96.34(14) . . ?
S3 P1 S1 117.06(6) 2_565 . ?
O1 P1 S2 113.52(12) . . ?
S3 P1 S2 109.58(6) 2_565 . ?
S1 P1 S2 108.98(6) . . ?
C11 P2 C17 103.09(17) . . ?
C11 P2 C5 105.87(18) . . ?
C17 P2 C5 101.10(18) . . ?
C11 P2 Cu1 109.20(13) . . ?
C17 P2 Cu1 118.79(13) . . ?
C5 P2 Cu1 117.22(12) . . ?
C29 P3 C23 103.05(19) . . ?
C29 P3 C35 105.67(17) . . ?
C23 P3 C35 101.52(18) . . ?
C29 P3 Cu2 113.96(14) . . ?
C23 P3 Cu2 119.88(13) . . ?
C35 P3 Cu2 111.18(13) . . ?
P1 S1 Cu1 114.55(5) . . ?
P1 S1 Cu2 82.12(4) . . ?
Cu1 S1 Cu2 70.10(3) . . ?
P1 S2 Cu1 88.31(5) . 2_565 ?
P1 S2 Cu2 82.19(5) . . ?
Cu1 S2 Cu2 105.92(4) 2_565 . ?
P1 S3 Cu2 113.70(6) 2_565 . ?
P1 S3 Cu1 78.33(4) 2_565 . ?
Cu2 S3 Cu1 64.86(3) . . ?
O1 C1 C4 105.1(4) . . ?
O1 C1 C3 111.3(4) . . ?
C4 C1 C3 113.0(5) . . ?
O1 C1 C2 106.5(4) . . ?
C4 C1 C2 107.6(5) . . ?
C3 C1 C2 112.8(5) . . ?
C10 C5 C6 119.5(4) . . ?
C10 C5 P2 125.3(3) . . ?
C6 C5 P2 114.9(3) . . ?
C5 C6 C7 119.8(4) . . ?
C8 C7 C6 119.9(5) . . ?
C7 C8 C9 120.4(5) . . ?
C8 C9 C10 119.8(4) . . ?
C5 C10 C9 120.6(4) . . ?
C16 C11 C12 118.9(4) . . ?
C16 C11 P2 119.2(3) . . ?
C12 C11 P2 121.5(3) . . ?
C13 C12 C11 120.0(4) . . ?
C14 C13 C12 121.1(5) . . ?
C15 C14 C13 119.0(4) . . ?
C14 C15 C16 120.6(4) . . ?
C11 C16 C15 120.4(4) . . ?
C22 C17 C18 119.0(4) . . ?
C22 C17 P2 119.2(3) . . ?
C18 C17 P2 121.7(3) . . ?
C19 C18 C17 120.0(4) . . ?
C20 C19 C18 120.5(4) . . ?
C21 C20 C19 119.7(4) . . ?
C20 C21 C22 120.3(4) . . ?
C21 C22 C17 120.4(4) . . ?
C24 C23 C28 119.1(4) . . ?
C24 C23 P3 117.2(3) . . ?
C28 C23 P3 123.6(3) . . ?
C25 C24 C23 119.8(5) . . ?
C26 C25 C24 120.5(5) . . ?
C27 C26 C25 120.5(5) . . ?
C26 C27 C28 120.1(5) . . ?
C27 C28 C23 119.9(5) . . ?
C30 C29 C34 118.3(4) . . ?
C30 C29 P3 124.7(3) . . ?
C34 C29 P3 116.9(3) . . ?
C29 C30 C31 121.3(4) . . ?
C32 C31 C30 119.4(4) . . ?
C31 C32 C33 120.2(4) . . ?
C32 C33 C34 120.4(5) . . ?
C33 C34 C29 120.4(5) . . ?
C36 C35 C40 119.2(4) . . ?
C36 C35 P3 122.7(3) . . ?
C40 C35 P3 117.9(3) . . ?
C35 C36 C37 120.5(4) . . ?
C38 C37 C36 119.8(5) . . ?
C39 C38 C37 120.1(4) . . ?
C38 C39 C40 120.6(4) . . ?
C39 C40 C35 119.8(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.449(5) . ?
O1 P1 1.592(3) . ?
Cu1 P2 2.2303(11) . ?
Cu1 S1 2.2794(12) . ?
Cu1 S2 2.3243(10) 2_565 ?
Cu1 S3 2.7210(12) . ?
Cu1 Cu2 2.7241(7) . ?
Cu2 P3 2.2479(11) . ?
Cu2 S3 2.3190(12) . ?
Cu2 S2 2.4538(12) . ?
Cu2 S1 2.4574(11) . ?
P1 S3 2.0292(15) 2_565 ?
P1 S1 2.0400(15) . ?
P1 S2 2.0410(13) . ?
P2 C11 1.836(4) . ?
P2 C17 1.836(4) . ?
P2 C5 1.841(4) . ?
P3 C29 1.828(4) . ?
P3 C23 1.829(4) . ?
P3 C35 1.836(4) . ?
S2 Cu1 2.3243(10) 2_565 ?
S3 P1 2.0292(15) 2_565 ?
C1 C4 1.487(6) . ?
C1 C3 1.504(7) . ?
C1 C2 1.569(9) . ?
C5 C10 1.379(6) . ?
C5 C6 1.394(6) . ?
C6 C7 1.407(7) . ?
C7 C8 1.372(7) . ?
C8 C9 1.388(8) . ?
C9 C10 1.391(6) . ?
C11 C16 1.392(6) . ?
C11 C12 1.393(6) . ?
C12 C13 1.391(7) . ?
C13 C14 1.387(7) . ?
C14 C15 1.379(7) . ?
C15 C16 1.398(7) . ?
C17 C22 1.389(5) . ?
C17 C18 1.397(5) . ?
C18 C19 1.384(6) . ?
C19 C20 1.383(7) . ?
C20 C21 1.377(6) . ?
C21 C22 1.388(6) . ?
C23 C24 1.398(6) . ?
C23 C28 1.405(6) . ?
C24 C25 1.395(7) . ?
C25 C26 1.376(9) . ?
C26 C27 1.375(9) . ?
C27 C28 1.402(7) . ?
C29 C30 1.390(5) . ?
C29 C34 1.400(6) . ?
C30 C31 1.401(6) . ?
C31 C32 1.380(7) . ?
C32 C33 1.384(7) . ?
C33 C34 1.391(7) . ?
C35 C36 1.393(6) . ?
C35 C40 1.403(5) . ?
C36 C37 1.397(6) . ?
C37 C38 1.393(8) . ?
C38 C39 1.376(7) . ?
C39 C40 1.399(5) . ?
