#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:09:25 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244011 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/27/7702774.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_7702774
loop_
_publ_author_name
'López-Sandoval, Horacio'
'Contreras, Rosalinda'
'Escuer, Albert'
'Vicente, Ramon'
'Bernès, Sylvain'
'Nöth, Heinrich'
'Jeffery Leigh, G.'
'Barba-Behrens, Noráh'
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of the
 triangulo-tricopper(ii) complex [Cu3(cpse)3(H2O)3]·8.5H2O
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2648
_journal_paper_doi               10.1039/b110915b
_journal_year                    2002
_chemical_formula_sum            'C36 H68 Cu3 N3 O20.5'
_chemical_formula_weight         1061.55
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '2001-05-08 l'
_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                   15.1559(1)
_cell_length_b                   15.1559(1)
_cell_length_c                   37.3630(7)
_cell_measurement_temperature    183(2)
_cell_volume                     7432.52(16)
_computing_molecular_graphics    'SHELXTL 5.10 (Sheldrick, 1998)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL 5.10 (Sheldrick, 1998)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector                 'Area CCD'
_diffrn_measured_fraction_theta_full 0.720
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14234
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_T_max  0.90769
_exptl_absorpt_correction_T_min  0.80545
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             3336
_exptl_crystal_preparation
;
Crystal mounted on glass fiber with perfluorpolyetheroil
;
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_coef       0.00015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0274
_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)+(0.0347P)²+8.2073P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                2745
_reflns_number_total             3010
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b110915b.txt
_cod_data_source_block           noeth48
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_hydrogens' value 'geom + difmap' was
changed to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        7432.51(14)
_cod_original_sg_symbol_H-M      R32
_cod_original_formula_sum        'C36 H68 Cu3 N3 O20.50'
_cod_database_code               7702774
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+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 0.79995(2) 0.47068(2) 0.104257(9) 0.02141(9) Uani 1 1 d .
N1 N 0.94852(16) 0.51837(15) 0.09571(6) 0.0221(5) Uani 1 1 d .
C1 C 0.9470(2) 0.6771(2) 0.10754(8) 0.0276(6) Uani 1 1 d .
C2 C 0.9943(2) 0.62728(19) 0.08516(9) 0.0277(6) Uani 1 1 d .
H2A H 0.9819 0.6320 0.0600 0.033 Uiso 1 1 calc R
H2B H 1.0673 0.6623 0.0890 0.033 Uiso 1 1 calc R
O2 O 0.99712(16) 0.76877(15) 0.11469(6) 0.0390(5) Uani 1 1 d .
O3 O 0.85427(13) 0.61657(14) 0.11721(5) 0.0272(4) Uani 1 1 d .
C3 C 0.94460(19) 0.45023(19) 0.06571(8) 0.0230(6) Uani 1 1 d .
H3A H 0.9155 0.4656 0.0448 0.028 Uiso 1 1 calc R
C4 C 0.86892(19) 0.34072(19) 0.07717(8) 0.0220(6) Uani 1 1 d .
H4A H 0.9003 0.3205 0.0960 0.026 Uiso 1 1 calc R
O4 O 0.77870(14) 0.33674(13) 0.09133(6) 0.0250(4) Uani 1 1 d .
C5 C 1.0484(2) 0.4653(2) 0.05451(9) 0.0327(7) Uani 1 1 d .
H5A H 1.0923 0.5349 0.0476 0.049 Uiso 1 1 calc R
H5B H 1.0397 0.4214 0.0347 0.049 Uiso 1 1 calc R
H5C H 1.0783 0.4489 0.0742 0.049 Uiso 1 1 calc R
O5 O 0.77005(14) 0.44081(14) 0.16563(5) 0.0307(5) Uani 1 1 d .
H51 H 0.7147 0.4223 0.1706 0.046 Uiso 1 1 d R
H52 H 0.8115 0.4818 0.1813 0.046 Uiso 1 1 d R
C6 C 0.9993(2) 0.5101(2) 0.12875(8) 0.0326(7) Uani 1 1 d .
H6A H 1.0697 0.5334 0.1238 0.049 Uiso 1 1 calc R
H6B H 0.9664 0.4403 0.1364 0.049 Uiso 1 1 calc R
H6C H 0.9945 0.5512 0.1473 0.049 Uiso 1 1 calc R
C7 C 0.8433(2) 0.26834(19) 0.04542(8) 0.0259(6) Uani 1 1 d .
C8 C 0.7776(2) 0.2631(2) 0.01856(9) 0.0327(7) Uani 1 1 d .
H8A H 0.7455 0.3014 0.0205 0.039 Uiso 1 1 calc R
C9 C 0.7590(2) 0.2011(2) -0.01137(9) 0.0420(8) Uani 1 1 d .
H9A H 0.7156 0.1991 -0.0293 0.050 Uiso 1 1 calc R
C10 C 0.8055(3) 0.1428(3) -0.01415(11) 0.0480(9) Uani 1 1 d .
H10A H 0.7942 0.1021 -0.0342 0.058 Uiso 1 1 calc R
C11 C 0.8688(3) 0.1450(3) 0.01279(11) 0.0470(9) Uani 1 1 d .
H11A H 0.8981 0.1040 0.0112 0.056 Uiso 1 1 calc R
C12 C 0.8891(2) 0.2082(2) 0.04240(9) 0.0337(7) Uani 1 1 d .
H12A H 0.9331 0.2104 0.0602 0.040 Uiso 1 1 calc R
O6 O 1.3333 0.6667 0.08437(15) 0.0875(17) Uani 1 3 d S
H61 H 1.3230 0.6179 0.0923 0.131 Uiso 0.67 1 d PR
O7 O 0.74771(19) 0.6667 0.1667 0.0415(8) Uani 1 2 d S
H71 H 0.8028 0.7192 0.1573 0.062 Uiso 1 1 d R
O8 O 1.21755(19) 0.9072(2) 0.11801(8) 0.0633(8) Uani 1 1 d .
H81 H 1.2375 0.9636 0.1346 0.095 Uiso 1 1 d R
H82 H 1.1446 0.8656 0.1154 0.095 Uiso 1 1 d R
O9 O 1.2535(3) 0.7490(3) 0.13270(14) 0.1240(17) Uani 1 1 d .
H92 H 1.2644 0.7292 0.1513 0.186 Uiso 1 1 d R
H91 H 1.2937 0.7296 0.1192 0.186 Uiso 1 1 d 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'
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
O4 Cu1 O4 95.86(11) . 2_655
O4 Cu1 O3 167.28(7) . .
O4 Cu1 O3 96.37(8) 2_655 .
O4 Cu1 N1 84.70(8) . .
O4 Cu1 N1 155.61(9) 2_655 .
O3 Cu1 N1 82.72(8) . .
O4 Cu1 O5 97.25(8) . .
O4 Cu1 O5 96.79(8) 2_655 .
O3 Cu1 O5 84.79(7) . .
N1 Cu1 O5 107.36(8) . .
C2 N1 C6 109.8(2) . .
C2 N1 C3 113.6(2) . .
C6 N1 C3 113.8(2) . .
C2 N1 Cu1 104.89(15) . .
C6 N1 Cu1 111.66(17) . .
C3 N1 Cu1 102.59(15) . .
O2 C1 O3 125.4(3) . .
O2 C1 C2 119.9(2) . .
O3 C1 C2 114.7(2) . .
N1 C2 C1 109.3(2) . .
C1 O3 Cu1 114.83(16) . .
N1 C3 C5 114.6(2) . .
N1 C3 C4 106.6(2) . .
C5 C3 C4 113.2(2) . .
O4 C4 C7 111.1(2) . .
O4 C4 C3 109.2(2) . .
C7 C4 C3 110.1(2) . .
C4 O4 Cu1 112.86(14) . .
C4 O4 Cu1 114.21(14) . 3_665
Cu1 O4 Cu1 131.12(10) . 3_665
C8 C7 C12 118.6(3) . .
C8 C7 C4 121.4(2) . .
C12 C7 C4 119.9(3) . .
C7 C8 C9 121.1(3) . .
C10 C9 C8 119.6(3) . .
C11 C10 C9 120.0(3) . .
C10 C11 C12 120.6(3) . .
C11 C12 C7 120.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 1.9504(17) .
Cu1 O4 1.9527(18) 2_655
Cu1 O3 1.9952(18) .
Cu1 N1 2.017(2) .
Cu1 O5 2.337(2) .
N1 C2 1.489(3) .
N1 C6 1.493(4) .
N1 C3 1.505(3) .
C1 O2 1.234(3) .
C1 O3 1.287(3) .
C1 C2 1.524(4) .
C3 C5 1.531(4) .
C3 C4 1.533(3) .
C4 O4 1.439(3) .
C4 C7 1.528(4) .
O4 Cu1 1.9527(18) 3_665
C7 C8 1.387(4) .
C7 C12 1.399(4) .
C8 C9 1.395(5) .
C9 C10 1.382(5) .
C10 C11 1.379(5) .
C11 C12 1.393(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_distance_DA
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
O5 H51 0.763 2.063 154.11 2.769 O5 2_655
O5 H52 0.857 1.879 175.33 2.734 O2 11_565
O6 H61 0.736 2.133 149.20 2.791 O9 2_755
O8 H81 0.974 2.031 156.47 2.949 O7 2_765
O8 H82 0.965 1.968 172.50 2.927 O2 1_555
O9 H91 0.944 1.880 161.34 2.791 O6 1_555
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
O4 Cu1 N1 C2 152.71(19) . .
O4 Cu1 N1 C2 60.2(3) 2_655 .
O3 Cu1 N1 C2 -29.13(17) . .
O5 Cu1 N1 C2 -111.33(17) . .
O4 Cu1 N1 C6 -88.45(18) . .
O4 Cu1 N1 C6 179.07(19) 2_655 .
O3 Cu1 N1 C6 89.71(18) . .
O5 Cu1 N1 C6 7.51(19) . .
O4 Cu1 N1 C3 33.76(16) . .
O4 Cu1 N1 C3 -58.7(3) 2_655 .
O3 Cu1 N1 C3 -148.08(17) . .
O5 Cu1 N1 C3 129.72(15) . .
C6 N1 C2 C1 -81.4(3) . .
C3 N1 C2 C1 150.0(2) . .
Cu1 N1 C2 C1 38.7(3) . .
O2 C1 C2 N1 150.1(3) . .
O3 C1 C2 N1 -30.5(4) . .
O2 C1 O3 Cu1 -175.5(3) . .
C2 C1 O3 Cu1 5.2(3) . .
O4 Cu1 O3 C1 22.8(5) . .
O4 Cu1 O3 C1 -141.0(2) 2_655 .
N1 Cu1 O3 C1 14.4(2) . .
O5 Cu1 O3 C1 122.7(2) . .
C2 N1 C3 C5 70.5(3) . .
C6 N1 C3 C5 -56.1(3) . .
Cu1 N1 C3 C5 -176.9(2) . .
C2 N1 C3 C4 -163.4(2) . .
C6 N1 C3 C4 70.0(3) . .
Cu1 N1 C3 C4 -50.8(2) . .
N1 C3 C4 O4 46.0(3) . .
C5 C3 C4 O4 173.0(2) . .
N1 C3 C4 C7 168.3(2) . .
C5 C3 C4 C7 -64.8(3) . .
C7 C4 O4 Cu1 -139.11(18) . .
C3 C4 O4 Cu1 -17.4(3) . .
C7 C4 O4 Cu1 54.5(3) . 3_665
C3 C4 O4 Cu1 176.15(18) . 3_665
O4 Cu1 O4 C4 145.88(15) 2_655 .
O3 Cu1 O4 C4 -18.0(5) . .
N1 Cu1 O4 C4 -9.62(18) . .
O5 Cu1 O4 C4 -116.49(18) . .
O4 Cu1 O4 Cu1 -50.6(2) 2_655 3_665
O3 Cu1 O4 Cu1 145.5(3) . 3_665
N1 Cu1 O4 Cu1 153.87(16) . 3_665
O5 Cu1 O4 Cu1 47.00(15) . 3_665
O4 C4 C7 C8 45.0(3) . .
C3 C4 C7 C8 -76.1(3) . .
O4 C4 C7 C12 -137.2(3) . .
C3 C4 C7 C12 101.7(3) . .
C12 C7 C8 C9 -1.5(4) . .
C4 C7 C8 C9 176.3(3) . .
C7 C8 C9 C10 1.0(5) . .
C8 C9 C10 C11 0.9(5) . .
C9 C10 C11 C12 -2.1(5) . .
C10 C11 C12 C7 1.5(5) . .
C8 C7 C12 C11 0.3(5) . .
C4 C7 C12 C11 -177.6(3) . .
