#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:18:40 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179530 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/27/4342705.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_4342705
loop_
_publ_author_name
'Spielberg, Eike T.'
'Gilb, Aksana'
'Plaul, Daniel'
'Geibig, Daniel'
'Hornig, David'
'Schuch, Dirk'
'Buchholz, Axel'
'Ardavan, Arzhang'
'Plass, Winfried'
_publ_section_title
;
 A spin-frustrated trinuclear copper complex based on triaminoguanidine
 with an energetically well-separated degenerate ground state.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3432
_journal_page_last               3438
_journal_paper_doi               10.1021/ic503095t
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C61 H60 Cl Cu3 N15 O10'
_chemical_formula_weight         1389.31
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.8205(11)
_cell_length_b                   19.8205(11)
_cell_length_c                   26.4663(15)
_cell_measurement_temperature    183(2)
_cell_volume                     9004.4(9)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13785
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         1.943
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             4290
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3091
_reflns_number_total             4219
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic503095t_si_002.cif
_cod_data_source_block           fo2164
_cod_depositor_comments          'Adding full bibliography for 4342705.cif.'
_cod_original_cell_volume        9004.4(13)
_cod_database_code               4342705
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.720
_shelx_estimated_absorpt_t_max   0.720
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu Cu 0.44145(3) 0.61658(3) 0.08557(2) 0.0394(2) Uani 1 1 d . . .
O1 O 0.54575(15) 0.64066(16) 0.10268(11) 0.0494(7) Uani 1 1 d . . .
N1 N 0.40114(17) 0.73523(18) 0.10005(11) 0.0389(7) Uani 1 1 d . . .
N2 N 0.46389(18) 0.72331(18) 0.09883(11) 0.0401(7) Uani 1 1 d . . .
N3 N 0.41997(17) 0.50901(18) 0.06473(11) 0.0400(7) Uani 1 1 d . . .
N4 N 0.43993(18) 0.62021(19) 0.00071(13) 0.0448(8) Uani 1 1 d . . .
C1 C 0.3333 0.6667 0.0998(2) 0.0366(13) Uani 1 3 d S T P
C2 C 0.5326(2) 0.7820(2) 0.10630(15) 0.0450(9) Uani 1 1 d . . .
H2 H 0.5361 0.8309 0.1126 0.054 Uiso 1 1 calc R U .
C3 C 0.6042(2) 0.7802(3) 0.10600(15) 0.0492(9) Uani 1 1 d . . .
C4 C 0.6744(3) 0.8521(3) 0.10878(19) 0.0624(12) Uani 1 1 d . . .
H4 H 0.6721 0.8989 0.1089 0.075 Uiso 1 1 calc R U .
C5 C 0.7442(3) 0.8568(3) 0.1113(2) 0.0639(13) Uani 1 1 d . . .
H5 H 0.7905 0.9062 0.1132 0.077 Uiso 1 1 calc R U .
C6 C 0.7482(3) 0.7886(3) 0.11124(18) 0.0587(11) Uani 1 1 d . . .
H6 H 0.7977 0.7919 0.1124 0.070 Uiso 1 1 calc R U .
C7 C 0.6819(3) 0.7166(3) 0.10945(16) 0.0540(11) Uani 1 1 d . . .
H7 H 0.6858 0.6707 0.1112 0.065 Uiso 1 1 calc R U .
C8 C 0.6074(2) 0.7105(2) 0.10506(14) 0.0453(9) Uani 1 1 d . . .
C9 C 0.4196(2) 0.4575(2) 0.09773(16) 0.0476(9) Uani 1 1 d . . .
H9 H 0.4320 0.4728 0.1320 0.057 Uiso 1 1 calc R U .
C10 C 0.4019(2) 0.3824(3) 0.08403(18) 0.0555(11) Uani 1 1 d . . .
H10 H 0.4004 0.3467 0.1086 0.067 Uiso 1 1 calc R U .
C11 C 0.3866(3) 0.3616(3) 0.0340(2) 0.0600(11) Uani 1 1 d . . .
H11 H 0.3739 0.3108 0.0234 0.072 Uiso 1 1 calc R U .
C12 C 0.3899(2) 0.4150(2) -0.00054(17) 0.0533(10) Uani 1 1 d . . .
H12 H 0.3805 0.4015 -0.0353 0.064 Uiso 1 1 calc R U .
C13 C 0.4071(2) 0.4889(2) 0.01557(14) 0.0430(9) Uani 1 1 d . . .
C14 C 0.4155(2) 0.5506(2) -0.02026(14) 0.0425(8) Uani 1 1 d . . .
C15 C 0.4024(3) 0.5372(3) -0.07151(15) 0.0538(10) Uani 1 1 d . . .
H15 H 0.3826 0.4865 -0.0853 0.065 Uiso 1 1 calc R U .
C16 C 0.4191(3) 0.6007(3) -0.10229(17) 0.0630(13) Uani 1 1 d . . .
H16 H 0.4117 0.5940 -0.1378 0.076 Uiso 1 1 calc R U .
C17 C 0.4460(3) 0.6721(3) -0.08152(17) 0.0607(12) Uani 1 1 d . . .
H17 H 0.4583 0.7161 -0.1021 0.073 Uiso 1 1 calc R U .
C18 C 0.4550(3) 0.6796(3) -0.02953(16) 0.0541(10) Uani 1 1 d . . .
H18 H 0.4728 0.7294 -0.0149 0.065 Uiso 1 1 calc R U .
Cl1 Cl 0.0000 0.0000 0.11258(7) 0.0573(5) Uani 1 3 d S T P
O11 O 0.0000 0.0000 0.0604(3) 0.168(5) Uani 1 3 d S T P
O12 O -0.0392(3) 0.0375(3) 0.1330(2) 0.1171(17) Uani 1 1 d . . .
N1D N 0.1083(4) 0.2660(4) -0.0619(3) 0.116(2) Uani 1 1 d . . .
O1D O 0.2217(4) 0.3800(4) -0.0790(5) 0.210(5) Uani 1 1 d . . .
C3D C 0.0878(4) 0.2623(5) -0.1166(3) 0.111(2) Uani 1 1 d . . .
H3A H 0.1282 0.3085 -0.1340 0.167 Uiso 0.5 1 calc R U P
H3B H 0.0376 0.2604 -0.1199 0.167 Uiso 0.5 1 calc R U P
H3C H 0.0840 0.2154 -0.1318 0.167 Uiso 0.5 1 calc R U P
H3D H 0.0383 0.2144 -0.1231 0.167 Uiso 0.5 1 calc R U P
H3E H 0.1289 0.2624 -0.1372 0.167 Uiso 0.5 1 calc R U P
H3F H 0.0826 0.3075 -0.1254 0.167 Uiso 0.5 1 calc R U P
C1D C 0.1817(5) 0.3325(6) -0.0476(4) 0.133(4) Uani 1 1 d . . .
H1A H 0.1987 0.3389 -0.0134 0.160 Uiso 1 1 calc R U .
C2D C 0.0585(7) 0.2051(7) -0.0292(4) 0.163(4) Uani 1 1 d . . .
H2A H 0.0135 0.1658 -0.0482 0.244 Uiso 0.5 1 calc R U P
H2B H 0.0404 0.2260 -0.0021 0.244 Uiso 0.5 1 calc R U P
H2C H 0.0868 0.1811 -0.0145 0.244 Uiso 0.5 1 calc R U P
H2D H 0.0803 0.2161 0.0050 0.244 Uiso 0.5 1 calc R U P
H2E H 0.0534 0.1559 -0.0411 0.244 Uiso 0.5 1 calc R U P
H2F H 0.0071 0.2008 -0.0288 0.244 Uiso 0.5 1 calc R U P
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'
Cl Cl 0.1484 0.1585 '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
O1 Cu N2 93.10(13) . .
O1 Cu N1 155.14(12) . 3_565
N2 Cu N1 78.71(13) . 3_565
O1 Cu N3 87.69(12) . .
N2 Cu N3 174.50(12) . .
N1 Cu N3 102.72(12) 3_565 .
O1 Cu N4 104.87(12) . .
N2 Cu N4 98.25(12) . .
N1 Cu N4 99.55(12) 3_565 .
N3 Cu N4 76.29(12) . .
C8 O1 Cu 126.1(2) . .
C1 N1 N2 110.9(2) . .
C1 N1 Cu 111.22(18) . 2_665
N2 N1 Cu 135.9(2) . 2_665
C2 N2 N1 118.6(3) . .
C2 N2 Cu 124.6(3) . .
N1 N2 Cu 116.8(2) . .
C9 N3 C13 118.4(3) . .
C9 N3 Cu 122.8(3) . .
C13 N3 Cu 118.9(3) . .
C14 N4 C18 118.1(4) . .
C14 N4 Cu 112.7(2) . .
C18 N4 Cu 129.0(3) . .
N1 C1 N1 119.998(6) 2_665 3_565
N1 C1 N1 119.997(6) 2_665 .
N1 C1 N1 119.999(6) 3_565 .
N2 C2 C3 126.0(4) . .
C4 C3 C8 119.0(4) . .
C4 C3 C2 117.6(4) . .
C8 C3 C2 123.4(4) . .
C5 C4 C3 122.3(4) . .
C4 C5 C6 119.3(4) . .
C7 C6 C5 121.3(4) . .
C6 C7 C8 120.1(4) . .
O1 C8 C3 123.9(3) . .
O1 C8 C7 118.1(4) . .
C3 C8 C7 117.9(4) . .
N3 C9 C10 123.1(4) . .
C11 C10 C9 118.1(4) . .
C10 C11 C12 119.4(4) . .
C11 C12 C13 119.8(4) . .
N3 C13 C12 121.1(4) . .
N3 C13 C14 116.4(3) . .
C12 C13 C14 122.4(4) . .
N4 C14 C15 122.9(4) . .
N4 C14 C13 114.7(3) . .
C15 C14 C13 122.3(4) . .
C14 C15 C16 117.6(4) . .
C17 C16 C15 119.9(4) . .
C16 C17 C18 118.5(4) . .
N4 C18 C17 123.0(4) . .
O11 Cl1 O12 112.3(2) . 2
O11 Cl1 O12 112.3(2) . 3
O12 Cl1 O12 106.5(2) 2 3
O11 Cl1 O12 112.3(2) . .
O12 Cl1 O12 106.5(2) 2 .
O12 Cl1 O12 106.5(2) 3 .
C2D N1D C1D 125.2(10) . .
C2D N1D C3D 119.6(8) . .
C1D N1D C3D 115.1(7) . .
O1D C1D N1D 120.0(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O1 1.929(3) .
Cu N2 1.963(3) .
Cu N1 2.013(3) 3_565
Cu N3 2.031(3) .
Cu N4 2.248(3) .
O1 C8 1.313(5) .
N1 C1 1.352(3) .
N1 N2 1.377(4) .
N1 Cu 2.013(3) 2_665
N2 C2 1.289(5) .
N3 C9 1.341(5) .
N3 C13 1.347(5) .
N4 C14 1.334(5) .
N4 C18 1.328(5) .
C1 N1 1.351(3) 2_665
C1 N1 1.351(3) 3_565
C2 C3 1.438(6) .
C3 C4 1.410(6) .
C3 C8 1.415(6) .
C4 C5 1.341(7) .
C5 C6 1.395(7) .
C6 C7 1.375(6) .
C7 C8 1.425(6) .
C9 C10 1.395(6) .
C10 C11 1.374(7) .
C11 C12 1.376(6) .
C12 C13 1.395(5) .
C13 C14 1.489(5) .
C14 C15 1.382(6) .
C15 C16 1.394(7) .
C16 C17 1.355(7) .
C17 C18 1.386(6) .
Cl1 O11 1.381(9) .
Cl1 O12 1.422(5) 2
Cl1 O12 1.422(5) 3
Cl1 O12 1.422(5) .
N1D C2D 1.411(12) .
N1D C1D 1.442(10) .
N1D C3D 1.498(10) .
O1D C1D 1.210(14) .
