#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:32:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179975 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/69/7026905.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_7026905
loop_
_publ_author_name
'Safin, Damir A.'
'Babashkina, Maria G.'
'Bolte, Michael'
'Pape, Tania'
'Hahn, F. Ekkehardt'
'Verizhnikov, Maxim L.'
'Bashirov, Airat R.'
'Klein, Axel'
_publ_section_title
;
 Polynuclear and mixed-ligand mononuclear Cu(I) complexes with
 N-thiophosphorylated thioureas and 1,10-phenanthroline or PPh3.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11577
_journal_page_last               11586
_journal_paper_doi               10.1039/c0dt00866d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C45 H72 Cu3 N6 O6 P3 S6'
_chemical_formula_sum            'C45 H72 Cu3 N6 O6 P3 S6'
_chemical_formula_weight         1268.98
_chemical_name_systematic        ?
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            6
_cell_length_a                   17.9577(7)
_cell_length_b                   17.9577(7)
_cell_length_c                   32.1945(17)
_cell_measurement_reflns_used    15044
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.6
_cell_volume                     8991.1(7)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16656
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         3.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  0.7052
_exptl_absorpt_correction_T_min  0.6646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3960
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0487P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                3247
_reflns_number_total             3745
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c0dt00866d.txt
_cod_data_source_block           safin27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7026905
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Cu1 Cu 0.468779(14) 0.772484(15) 0.425221(8) 0.02271(9) Uani 1 1 d .
P1 P 0.64291(3) 0.78033(3) 0.430287(16) 0.01749(12) Uani 1 1 d .
S1 S 0.60295(3) 0.85424(3) 0.403349(18) 0.02574(13) Uani 1 1 d .
S2 S 0.43328(3) 0.63730(3) 0.439480(18) 0.02398(13) Uani 1 1 d .
N1 N 0.59682(10) 0.68110(10) 0.41707(5) 0.0207(3) Uani 1 1 d .
N2 N 0.49016(11) 0.54356(10) 0.40374(6) 0.0236(4) Uani 1 1 d .
H2 H 0.4374(17) 0.5061(16) 0.4091(8) 0.034(7) Uiso 1 1 d .
O1 O 0.74146(8) 0.81889(8) 0.42044(4) 0.0208(3) Uani 1 1 d .
O2 O 0.64198(9) 0.78289(8) 0.47884(4) 0.0242(3) Uani 1 1 d .
C1 C 0.51562(11) 0.62298(12) 0.41862(6) 0.0194(4) Uani 1 1 d .
C2 C 0.77432(13) 0.83831(14) 0.37789(7) 0.0262(4) Uani 1 1 d .
H2A H 0.7260 0.8255 0.3584 0.031 Uiso 1 1 calc R
C3 C 0.81185(15) 0.78221(17) 0.36737(8) 0.0370(5) Uani 1 1 d .
H3A H 0.7665 0.7217 0.3683 0.055 Uiso 1 1 calc R
H3B H 0.8568 0.7921 0.3875 0.055 Uiso 1 1 calc R
H3C H 0.8368 0.7963 0.3394 0.055 Uiso 1 1 calc R
C4 C 0.83932(18) 0.93287(16) 0.37639(10) 0.0515(7) Uani 1 1 d .
H4A H 0.8111 0.9660 0.3832 0.077 Uiso 1 1 calc R
H4B H 0.8640 0.9482 0.3484 0.077 Uiso 1 1 calc R
H4C H 0.8851 0.9459 0.3966 0.077 Uiso 1 1 calc R
C5 C 0.68203(15) 0.86482(14) 0.50192(7) 0.0332(5) Uani 1 1 d .
H5 H 0.7015 0.9134 0.4818 0.040 Uiso 1 1 calc R
C6 C 0.75880(19) 0.8726(2) 0.52436(10) 0.0570(8) Uani 1 1 d .
H6A H 0.8002 0.8739 0.5041 0.085 Uiso 1 1 calc R
H6B H 0.7405 0.8231 0.5429 0.085 Uiso 1 1 calc R
H6C H 0.7858 0.9257 0.5407 0.085 Uiso 1 1 calc R
C7 C 0.6143(2) 0.8633(2) 0.52961(11) 0.0721(11) Uani 1 1 d .
H7A H 0.5666 0.8581 0.5126 0.108 Uiso 1 1 calc R
H7B H 0.6389 0.9168 0.5457 0.108 Uiso 1 1 calc R
H7C H 0.5931 0.8142 0.5486 0.108 Uiso 1 1 calc R
C11 C 0.54847(12) 0.51295(12) 0.39467(7) 0.0217(4) Uani 1 1 d .
C12 C 0.54759(14) 0.45094(13) 0.42111(7) 0.0279(5) Uani 1 1 d .
C13 C 0.60775(16) 0.42473(14) 0.41349(8) 0.0353(5) Uani 1 1 d .
H13 H 0.6094 0.3831 0.4311 0.042 Uiso 1 1 calc R
C14 C 0.66441(15) 0.45835(15) 0.38091(9) 0.0381(6) Uani 1 1 d .
H14 H 0.7060 0.4411 0.3767 0.046 Uiso 1 1 calc R
C15 C 0.66145(14) 0.51671(14) 0.35435(8) 0.0325(5) Uani 1 1 d .
H15 H 0.7003 0.5384 0.3316 0.039 Uiso 1 1 calc R
C16 C 0.60241(12) 0.54453(12) 0.36021(7) 0.0240(4) Uani 1 1 d .
C17 C 0.48418(19) 0.41286(17) 0.45630(8) 0.0457(6) Uani 1 1 d .
H17A H 0.4864 0.4592 0.4733 0.069 Uiso 1 1 calc R
H17B H 0.4988 0.3770 0.4735 0.069 Uiso 1 1 calc R
H17C H 0.4261 0.3776 0.4450 0.069 Uiso 1 1 calc R
C18 C 0.59636(15) 0.60335(14) 0.32904(7) 0.0330(5) Uani 1 1 d .
H18A H 0.6258 0.6623 0.3398 0.050 Uiso 1 1 calc R
H18B H 0.5358 0.5849 0.3239 0.050 Uiso 1 1 calc R
H18C H 0.6236 0.6013 0.3030 0.050 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'
Cu Cu 0.3201 1.2651 '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'
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
S2 Cu1 S1 134.34(2) 2_665 .
S2 Cu1 S2 111.30(2) 2_665 .
S1 Cu1 S2 114.269(19) . .
O2 P1 O1 102.36(8) . .
O2 P1 N1 106.92(8) . .
O1 P1 N1 106.09(8) . .
O2 P1 S1 113.72(6) . .
O1 P1 S1 108.57(6) . .
N1 P1 S1 117.83(7) . .
P1 S1 Cu1 93.13(2) . .
C1 S2 Cu1 113.43(7) . 3_565
C1 S2 Cu1 106.12(7) . .
Cu1 S2 Cu1 120.27(2) 3_565 .
C1 N1 P1 129.04(14) . .
C1 N2 C11 123.40(16) . .
C1 N2 H2 114.4(17) . .
C11 N2 H2 118.0(17) . .
C2 O1 P1 121.55(12) . .
C5 O2 P1 121.71(14) . .
N1 C1 N2 119.03(17) . .
N1 C1 S2 125.78(15) . .
N2 C1 S2 115.18(13) . .
O1 C2 C3 108.27(17) . .
O1 C2 C4 106.95(19) . .
C3 C2 C4 113.2(2) . .
O1 C2 H2A 109.4 . .
C3 C2 H2A 109.4 . .
C4 C2 H2A 109.4 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O2 C5 C7 107.2(2) . .
O2 C5 C6 107.58(19) . .
C7 C5 C6 114.6(3) . .
O2 C5 H5 109.1 . .
C7 C5 H5 109.1 . .
C6 C5 H5 109.1 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C16 C11 C12 122.59(18) . .
C16 C11 N2 119.87(18) . .
C12 C11 N2 117.54(19) . .
C11 C12 C13 117.3(2) . .
C11 C12 C17 121.7(2) . .
C13 C12 C17 121.0(2) . .
C14 C13 C12 120.9(2) . .
C14 C13 H13 119.6 . .
C12 C13 H13 119.6 . .
C13 C14 C15 120.5(2) . .
C13 C14 H14 119.7 . .
C15 C14 H14 119.7 . .
C14 C15 C16 121.1(2) . .
C14 C15 H15 119.5 . .
C16 C15 H15 119.5 . .
C15 C16 C11 117.4(2) . .
C15 C16 C18 119.9(2) . .
C11 C16 C18 122.61(18) . .
C12 C17 H17A 109.5 . .
C12 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C12 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 S2 2.1957(5) 2_665
Cu1 S1 2.2180(5) .
Cu1 S2 2.2277(5) .
P1 O2 1.5642(15) .
P1 O1 1.5768(13) .
P1 N1 1.6021(16) .
P1 S1 1.9952(7) .
S2 C1 1.7560(19) .
S2 Cu1 2.1958(5) 3_565
N1 C1 1.302(2) .
N2 C1 1.349(3) .
N2 C11 1.435(2) .
N2 H2 0.86(3) .
O1 C2 1.463(3) .
O2 C5 1.475(2) .
C2 C3 1.504(3) .
C2 C4 1.505(3) .
C2 H2A 1.0000 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C7 1.498(4) .
C5 C6 1.500(4) .
C5 H5 1.0000 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C11 C16 1.393(3) .
C11 C12 1.395(3) .
C12 C13 1.399(3) .
C12 C17 1.506(3) .
C13 C14 1.373(4) .
C13 H13 0.9500 .
C14 C15 1.374(4) .
C14 H14 0.9500 .
C15 C16 1.392(3) .
C15 H15 0.9500 .
C16 C18 1.500(3) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 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
N2 H2 S1 0.86(3) 2.92(3) 3.7465(17) 163(2) 3_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 P1 S1 Cu1 -67.91(6) . .
O1 P1 S1 Cu1 178.87(6) . .
N1 P1 S1 Cu1 58.34(8) . .
S2 Cu1 S1 P1 152.57(3) 2_665 .
S2 Cu1 S1 P1 -23.50(3) . .
S2 Cu1 S2 C1 170.26(7) 2_665 .
S1 Cu1 S2 C1 -12.76(7) . .
S2 Cu1 S2 Cu1 39.88(5) 2_665 3_565
S1 Cu1 S2 Cu1 -143.14(3) . 3_565
O2 P1 N1 C1 72.6(2) . .
O1 P1 N1 C1 -178.70(18) . .
S1 P1 N1 C1 -56.9(2) . .
O2 P1 O1 C2 -172.67(13) . .
N1 P1 O1 C2 75.41(15) . .
S1 P1 O1 C2 -52.14(14) . .
O1 P1 O2 C5 66.62(16) . .
N1 P1 O2 C5 177.92(15) . .
S1 P1 O2 C5 -50.27(16) . .
P1 N1 C1 N2 176.60(16) . .
P1 N1 C1 S2 -4.4(3) . .
C11 N2 C1 N1 14.4(3) . .
C11 N2 C1 S2 -164.71(16) . .
Cu1 S2 C1 N1 169.09(16) 3_565 .
Cu1 S2 C1 N1 34.9(2) . .
Cu1 S2 C1 N2 -11.91(18) 3_565 .
Cu1 S2 C1 N2 -146.10(14) . .
P1 O1 C2 C3 -117.00(17) . .
P1 O1 C2 C4 120.70(17) . .
P1 O2 C5 C7 124.4(2) . .
P1 O2 C5 C6 -111.9(2) . .
C1 N2 C11 C16 -72.3(3) . .
C1 N2 C11 C12 108.5(2) . .
C16 C11 C12 C13 4.2(3) . .
N2 C11 C12 C13 -176.61(18) . .
C16 C11 C12 C17 -175.3(2) . .
N2 C11 C12 C17 3.9(3) . .
C11 C12 C13 C14 -0.8(3) . .
C17 C12 C13 C14 178.8(2) . .
C12 C13 C14 C15 -1.9(4) . .
C13 C14 C15 C16 1.3(3) . .
C14 C15 C16 C11 1.9(3) . .
C14 C15 C16 C18 -175.6(2) . .
C12 C11 C16 C15 -4.7(3) . .
N2 C11 C16 C15 176.06(18) . .
C12 C11 C16 C18 172.7(2) . .
N2 C11 C16 C18 -6.5(3) . .
