#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:11:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179956 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/51/7025155.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_7025155
loop_
_publ_author_name
'Babashkina, Maria G.'
'Safin, Damir A.'
'Fayon, Franck'
'Rakhmatullin, Aydar I.'
'Sokolov, Felix D.'
'Klein, Axel'
'Krivolapov, Dmitriy B.'
'Pape, Tania'
'Hahn, F. Ekkehardt'
'Kozlowski, Henryk'
_publ_section_title
;
 Copper(I) complexes with N-(diisopropoxythiophosphoryl)thiobenzamide
 PhC(S)NHP(S)(OiPr)2.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8261
_journal_page_last               8268
_journal_paper_doi               10.1039/b925478a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C50 H72 Cu4 N4 O8 P4 S8'
_chemical_formula_sum            'C50 H72 Cu4 N4 O8 P4 S8'
_chemical_formula_weight         1491.74
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 112.45(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.26(2)
_cell_length_b                   11.370(10)
_cell_length_c                   26.80(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      2.4
_cell_volume                     7395(11)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        process_MolEN_(Fair,_1990)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    ' Direct_methods_(SIR,_Burla_et_al.,_1989)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.695
_diffrn_measured_fraction_theta_max 0.695
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2442
_diffrn_reflns_av_sigmaI/netI    0.3663
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7826
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.36
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.2750
_refine_ls_R_factor_gt           0.0693
_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)+(0.0779P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1903
_reflns_number_gt                1248
_reflns_number_total             3697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b925478a.txt
_cod_data_source_block           '[Cu4L4]'
_cod_original_cell_volume        7395(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7025155
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
C1 C 1.1336(5) 0.3087(15) 0.2965(5) 0.064(6) Uani 1 1 d .
C2 C 1.1638(6) 0.3332(15) 0.3635(6) 0.063(6) Uani 1 1 d .
C3 C 1.2161(6) 0.3568(14) 0.3856(6) 0.060(6) Uani 1 1 d .
H3 H 1.2367 0.3584 0.3641 0.072 Uiso 1 1 calc R
C4 C 1.2441(6) 0.3816(16) 0.4450(7) 0.080(6) Uani 1 1 d .
H4 H 1.2822 0.3918 0.4591 0.097 Uiso 1 1 calc R
C5 C 1.2161(7) 0.3904(18) 0.4809(6) 0.090(7) Uani 1 1 d .
H5 H 1.2343 0.4122 0.5168 0.108 Uiso 1 1 calc R
C6 C 1.1633(7) 0.3664(16) 0.4610(6) 0.078(7) Uani 1 1 d .
H6 H 1.1429 0.3688 0.4828 0.094 Uiso 1 1 calc R
C7 C 1.1355(5) 0.3339(14) 0.4006(6) 0.064(5) Uani 1 1 d .
H7 H 1.0984 0.3135 0.3872 0.077 Uiso 1 1 calc R
C8 C 1.0465(8) 0.4627(19) 0.1172(9) 0.106(7) Uani 1 1 d .
H8 H 1.0452 0.3927 0.0954 0.127 Uiso 1 1 calc R
C9 C 1.0522(10) 0.565(3) 0.0874(10) 0.249(18) Uani 1 1 d .
H9A H 1.0840 0.5561 0.0782 0.374 Uiso 1 1 calc R
H9B H 1.0566 0.6344 0.1093 0.374 Uiso 1 1 calc R
H9C H 1.0199 0.5735 0.0549 0.374 Uiso 1 1 calc R
C10 C 0.9989(9) 0.464(4) 0.1291(11) 0.36(3) Uani 1 1 d .
H10A H 0.9980 0.3944 0.1492 0.539 Uiso 1 1 calc R
H10B H 0.9669 0.4655 0.0961 0.539 Uiso 1 1 calc R
H10C H 0.9992 0.5323 0.1502 0.539 Uiso 1 1 calc R
C11 C 1.2127(8) 0.511(3) 0.2003(9) 0.125(10) Uani 1 1 d .
H11 H 1.1917 0.5503 0.2189 0.150 Uiso 1 1 calc R
C12 C 1.2138(11) 0.595(2) 0.1554(11) 0.227(11) Uani 1 1 d .
H12A H 1.1767 0.6150 0.1322 0.340 Uiso 1 1 calc R
H12B H 1.2319 0.5575 0.1347 0.340 Uiso 1 1 calc R
H12C H 1.2334 0.6657 0.1715 0.340 Uiso 1 1 calc R
C13 C 1.2649(12) 0.479(3) 0.2407(10) 0.227(11) Uani 1 1 d .
H13A H 1.2591 0.4298 0.2673 0.340 Uiso 1 1 calc R
H13B H 1.2847 0.5481 0.2577 0.340 Uiso 1 1 calc R
H13C H 1.2859 0.4358 0.2242 0.340 Uiso 1 1 calc R
C14 C 1.0170(6) -0.0826(17) 0.3916(5) 0.072(7) Uani 1 1 d .
C15 C 0.9741(6) -0.1034(14) 0.4177(7) 0.053(5) Uani 1 1 d .
C16 C 0.9924(6) -0.1440(13) 0.4765(6) 0.057(5) Uani 1 1 d .
H16 H 1.0295 -0.1609 0.4953 0.068 Uiso 1 1 calc R
C17 C 0.9554(8) -0.1575(17) 0.5043(7) 0.094(7) Uani 1 1 d .
H17 H 0.9669 -0.1745 0.5409 0.113 Uiso 1 1 calc R
C18 C 0.9025(8) -0.1427(17) 0.4714(9) 0.093(7) Uani 1 1 d .
H18 H 0.8753 -0.1545 0.4853 0.112 Uiso 1 1 calc R
C19 C 0.8847(6) -0.1071(16) 0.4117(9) 0.091(6) Uani 1 1 d .
H19 H 0.8473 -0.0960 0.3917 0.109 Uiso 1 1 calc R
C21 C 1.1299(14) -0.250(4) 0.3084(13) 0.088(6) Uani 0.50 1 d PD
H21 H 1.1650 -0.2083 0.3230 0.105 Uiso 0.50 1 calc PR
C22 C 1.1140(18) -0.225(5) 0.2586(18) 0.236(15) Uani 0.50 1 d P
H22A H 1.1043 -0.1437 0.2534 0.353 Uiso 0.50 1 calc PR
H22B H 1.0825 -0.2726 0.2385 0.353 Uiso 0.50 1 calc PR
H22C H 1.1432 -0.2413 0.2464 0.353 Uiso 0.50 1 calc PR
C23 C 1.1436(11) -0.347(3) 0.3281(9) 0.236(15) Uani 1 1 d .
H23A H 1.1500 -0.3442 0.3658 0.353 Uiso 1 1 calc R
H23B H 1.1768 -0.3704 0.3238 0.353 Uiso 1 1 calc R
H23C H 1.1149 -0.4025 0.3103 0.353 Uiso 1 1 calc R
C24 C 1.1581(7) -0.230(2) 0.5127(7) 0.088(6) Uani 1 1 d .
H24 H 1.1339 -0.1735 0.5207 0.105 Uiso 1 1 calc R
C25 C 1.2152(7) -0.224(2) 0.5586(8) 0.173(12) Uani 1 1 d .
H25A H 1.2301 -0.1461 0.5604 0.260 Uiso 1 1 calc R
H25B H 1.2393 -0.2797 0.5519 0.260 Uiso 1 1 calc R
H25C H 1.2120 -0.2422 0.5923 0.260 Uiso 1 1 calc R
C26 C 1.1344(8) -0.344(2) 0.5084(8) 0.140(9) Uani 1 1 d .
H26A H 1.0989 -0.3445 0.4793 0.210 Uiso 1 1 calc R
H26B H 1.1303 -0.3632 0.5415 0.210 Uiso 1 1 calc R
H26C H 1.1580 -0.4004 0.5014 0.210 Uiso 1 1 calc R
C20 C 0.9209(7) -0.0903(18) 0.3856(6) 0.099(8) Uani 1 1 d .
H20 H 0.9092 -0.0717 0.3491 0.118 Uiso 1 1 calc R
N1 N 1.1575(4) 0.3498(12) 0.2633(4) 0.064(5) Uani 1 1 d .
N2 N 1.0625(4) -0.1307(13) 0.4185(4) 0.067(5) Uani 1 1 d .
O1 O 1.0908(4) 0.4429(11) 0.1737(4) 0.076(4) Uani 1 1 d .
O2 O 1.1830(4) 0.4021(13) 0.1764(4) 0.082(4) Uani 1 1 d .
O3 O 1.1041(4) -0.2123(13) 0.3463(5) 0.132(6) Uani 1 1 d D
O4 O 1.1591(4) -0.1984(15) 0.4566(5) 0.155(8) Uani 1 1 d .
P1 P 1.13587(19) 0.3496(5) 0.19138(16) 0.0677(17) Uani 1 1 d .
P2 P 1.11740(17) -0.1275(6) 0.40530(18) 0.081(2) Uani 1 1 d .
S1 S 1.11563(16) 0.2031(5) 0.14689(15) 0.0779(17) Uani 1 1 d .
S2 S 1.06995(13) 0.2486(5) 0.27378(14) 0.0641(15) Uani 1 1 d .
S3 S 1.14948(14) 0.0214(5) 0.39996(17) 0.0864(18) Uani 1 1 d .
S4 S 0.99874(13) 0.0023(4) 0.32596(14) 0.0599(15) Uani 1 1 d .
Cu1 Cu 1.06061(6) 0.1451(2) 0.19087(6) 0.0673(9) Uani 1 1 d .
Cu2 Cu 1.07375(6) 0.0920(2) 0.33016(6) 0.0640(8) 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'
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'
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
N1 C1 C2 119.7(12) . .
N1 C1 S2 123.1(10) . .
C2 C1 S2 116.6(10) . .
C3 C2 C7 114.6(13) . .
C3 C2 C1 120.2(12) . .
C7 C2 C1 125.1(12) . .
C2 C3 C4 121.7(13) . .
C5 C4 C3 124.0(13) . .
C6 C5 C4 116.9(14) . .
C5 C6 C7 118.6(13) . .
C2 C7 C6 123.9(12) . .
C10 C8 C9 114(2) . .
C10 C8 O1 100.6(19) . .
C9 C8 O1 117.5(19) . .
C13 C11 O2 108(2) . .
C13 C11 C12 117(2) . .
O2 C11 C12 110.3(17) . .
N2 C14 C15 111.6(13) . .
N2 C14 S4 126.8(10) . .
C15 C14 S4 121.6(11) . .
C20 C15 C16 122.3(13) . .
C20 C15 C14 116.8(14) . .
C16 C15 C14 120.8(13) . .
C17 C16 C15 123.7(14) . .
C18 C17 C16 112.4(16) . .
C17 C18 C19 122.8(15) . .
C20 C19 C18 124.3(14) . .
C23 C21 C22 126(4) . .
C23 C21 O3 96(2) . .
C22 C21 O3 127(4) . .
C26 C24 C25 111.6(19) . .
C26 C24 O4 107.3(18) . .
C25 C24 O4 113.0(14) . .
C15 C20 C19 114.0(15) . .
C1 N1 P1 132.2(9) . .
C14 N2 P2 126.7(11) . .
P1 O1 C8 128.1(11) . .
C11 O2 P1 123.5(12) . .
C21 O3 P2 141.7(17) . .
C24 O4 P2 133.0(9) . .
O1 P1 O2 104.6(7) . .
O1 P1 N1 103.0(6) . .
O2 P1 N1 108.7(5) . .
O1 P1 S1 113.3(5) . .
O2 P1 S1 102.8(6) . .
N1 P1 S1 123.1(5) . .
N2 P2 O4 100.1(6) . .
N2 P2 O3 107.2(6) . .
O4 P2 O3 109.2(8) . .
N2 P2 S3 119.4(6) . .
O4 P2 S3 109.3(6) . .
O3 P2 S3 110.9(5) . .
P1 S1 Cu1 90.54(19) . .
C1 S2 Cu2 106.6(6) . .
C1 S2 Cu1 105.3(5) . .
Cu2 S2 Cu1 100.8(2) . .
P2 S3 Cu2 95.8(2) . .
C14 S4 Cu1 118.6(5) . 2_755
C14 S4 Cu2 106.6(5) . .
Cu1 S4 Cu2 102.9(2) 2_755 .
S4 Cu1 S1 130.79(17) 2_755 .
S4 Cu1 S2 111.30(15) 2_755 .
S1 Cu1 S2 117.83(17) . .
S4 Cu2 S3 111.27(19) . .
S4 Cu2 S2 120.88(16) . .
S3 Cu2 S2 127.61(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.352(14) .
C1 C2 1.687(18) .
C1 S2 1.690(14) .
C2 C3 1.300(15) .
C2 C7 1.450(16) .
C3 C4 1.502(17) .
C4 C5 1.421(18) .
C5 C6 1.311(17) .
C6 C7 1.544(17) .
C8 C10 1.40(2) .
C8 C9 1.46(3) .
C8 O1 1.533(19) .
C11 C13 1.43(3) .
C11 O2 1.47(2) .
C11 C12 1.55(3) .
C14 N2 1.260(15) .
C14 C15 1.555(17) .
C14 S4 1.900(15) .
C15 C20 1.340(16) .
C15 C16 1.532(17) .
C16 C17 1.442(17) .
C17 C18 1.342(19) .
C18 C19 1.54(2) .
C19 C20 1.392(19) .
C21 C23 1.21(4) .
C21 C22 1.27(4) .
C21 O3 1.483(10) .
C24 C26 1.42(2) .
C24 C25 1.54(2) .
C24 O4 1.556(17) .
N1 P1 1.790(11) .
N2 P2 1.609(11) .
O1 P1 1.523(12) .
O2 P1 1.558(10) .
O3 P2 1.770(14) .
O4 P2 1.610(11) .
P1 S1 1.999(7) .
P2 S3 1.920(8) .
S1 Cu1 2.283(4) .
S2 Cu2 2.312(5) .
S2 Cu1 2.442(5) .
S3 Cu2 2.293(5) .
S4 Cu1 2.175(5) 2_755
S4 Cu2 2.183(4) .
Cu1 S4 2.175(5) 2_755
